Effect of lanthanide contraction on the mixed polyamine systems Ln/Sb/Se/(en+dien) and Ln/Sb/Se/(en+trien): Syntheses and characterizations of lanthanide complexes with a tetraelenidoantimonate ligand

International Nuclear Information System (INIS)

Zhao Jing; Liang Jingjing; Pan Yingli; Zhang Yong; Jia Dingxian

2011-01-01

Mixed polyamine systems Ln/Sb/Se/(en+dien) and Ln/Sb/Se/(en+trien) (Ln=lanthanide, en=ethylenediamine, dien=diethylenetriamine, trien=triethylenetetramine) were investigated under solvothermal conditions, and novel mixed-coordinated lanthanide(III) complexes [Ln(en) 2 (dien)(η 2 -SbSe 4 )] (Ln=Ce(1a), Nd(1b)), [Ln(en) 2 (dien)(SbSe 4 )] (Ln=Sm(2a), Gd(2b), Dy(2c)), [Ln(en)(trien)(μ-η 1 ,η 2 -SbSe 4 )] ∞ (Ln=Ce(3a), Nd(3b)) and [Sm(en)(trien)(η 2 -SbSe 4 )] (4a) were prepared. Two structural types of lanthanide selenidoantimonates were obtained across the lanthanide series in both en+dien and en+trien systems. The tetrahedral anion [SbSe 4 ] 3- acts as a monodentate ligand mono-SbSe 4 , a bidentate chelating ligand η 2 -SbSe 4 or a tridentate bridging ligand μ-η 1 ,η 2 -SbSe 4 to the lanthanide(III) center depending on the Ln 3+ ions and the mixed ethylene polyamines, indicating the effect of lanthanide contraction on the structures of the lanthanide(III) selenidoantimonates. The lanthanide selenidoantimonates exhibit semiconducting properties with E g between 2.08 and 2.51 eV. - Graphical Abstract: Two structural types of lanthanide(III) selenidoantimonates are formed in both en-dien and en-trien mixed polyamines across lanthanide series, indicating the lanthanide contraction effect on the structures of the lanthanide(III) selenidoantimonates. Highlights: → Two structural types of lanthanide selenidoantimonates are prepared across the lanthanide series in both Ln/Sb/Se/(en+dien) and Ln/Sb/Se/(en+trien) systems. → The [SbSe 4 ] 3- anion acts as a mono-SbSe 4 , a η 2 -SbSe 4 or a μ-η 1 ,η 2 -SbSe 4 ligand to the Ln 3+ ions. → The soft base ligand [SbSe 4 ] 3- can be controlled to coordinate to the Ln 3+ ions with en+dien and en+trien as co-ligands.

Lanthanide (III) complexes of 2-(N-salicylideneamino)-4-phenylthiazole

International Nuclear Information System (INIS)

Sasidharan, G.N.; Mohanan, K.; Lakshmi Prabha, A.N.

2002-01-01

Lanthanide(III) complexes of 2-(N-salicylideneamino)-4- phenylthiazole (HSAT) have been synthesised and characterised by elemental, analytical, thermogravimetric, molar conductance, UV- visible, IR and NMR spectral data. The ligand coordinates to the lanthanide(III) ion in a tridentate fashion without deprotonation, giving complexes of the type [Ln(HSAT) 2 (NO 3 ) 3 ] and [Ln(HSAT) 2 (H 2 0) 3 Cl 3 ]. The spectral data reveal that the ligand is bonded to the lanthanide ion through azomethine nitrogen, ring nitrogen and phenolic oxygen without deprotonation. The nitrate group acts in a bidentate fashion. The ligand and the metal complexes exhibit antibacterial and antifungal activities. (author)

Complexation of f elements by tripodal ligands containing aromatic nitrogens. Application to the selective extraction of actinides(III)

International Nuclear Information System (INIS)

Wietzke, Raphael

1999-01-01

This work initiates a research project, whose aim is the actinides(lll)/lanthanides(III) separation by liquid-liquid extraction. We were interested in the study of the coordination chemistry of lanthanides(III) and uranium(III) (uranium(III) as model for the actinides(III)), with the aim to show differences between the two families and to better understand the coordination properties involved in the extraction process. We studied the lanthanide(III) and uranium(III) complexation with tripodal ligands containing aromatic nitrogens. Several tripodal ligands were synthesized varying the type and the number of the donor atoms. The lanthanide(III) complexes have been characterized in the solid state and in solution (by several techniques: "1H NMR, ESMS, luminescence, UV spectrophotometry, conductometry). Differences in the coordination were found depending on the nature of the donor atoms. The new ligands, tris(2-pyrazinylmethyl)amine (tpza) et tris(N,N-diethyl-2-carbamoyl-6- pyridylmethyl)amine (tpaa), have shown a selectivity for the actinides(III) with promising results in liquid-liquid extraction. The comparison between the lanthanum(III) and uranium(III) complexes with the ligand tpza showed differences in the bonding nature, which could be attributed to a covalent contribution to the metal-ligand bond. (author) [fr

Lanthanide(III) complexes of a mono(methylphosphonate) analogue of H4dota: the influence of protonation of the phosphonate moiety on the TSAP/SAP isomer ratio and the water exchange rate.

Science.gov (United States)

Rudovský, Jakub; Cígler, Petr; Kotek, Jan; Hermann, Petr; Vojtísek, Pavel; Lukes, Ivan; Peters, Joop A; Vander Elst, Luce; Muller, Robert N

2005-04-08

A monophosphonate analogue of H4dota, 1,4,7,10-tetraazacyclododecane-4,7,10-tris(carboxymethyl)-1-methylphosphonic acid (H5do3aP), and its complexes with lanthanides were synthesized. Multinuclear NMR studies reveal that, in aqueous solution, lanthanide(III) complexes of the ligand exhibit structures analogous to those of H4dota complexes. Thus, the central ion is nine-coordinate, surrounded by four nitrogen atoms, three acetate and one phosphonate oxygen atoms, and one water molecule in an apical position. For complexes of H5do3aP with Ln(III) ions in the middle of the series, the abundance of the desired twisted square-antiprismatic (TSAP) isomer is higher than for the corresponding H4dota complexes. The TSAP/square-antiprismatic (SAP) isomer ratio is highly sensitive to protonation of the phosphonate group: a higher abundance of the TSAP isomer was found in acidic solutions. The microscopic protonation constants of the TSAP isomers are higher than those of the SAP isomers. The presence of one water molecule in the first coordination sphere of the complexes in the pH region studied (pH 2.5-7.0) is confirmed by 17O NMR spectroscopy. The results of a simultaneous fit of variable-temperature 17O NMR relaxation data and 1H NMRD profiles show that the residence time of water (tauM) in the Gd(III) complex is much smaller than for [Gd(dota)(H2O)]-. The exchange rate appears to be dependent on the pH of the solution. The values of tauM are 37, 40, and 14 ns at pH 2.5, 4.7, and 7.0, respectively. These observations can be explained by an extensive second-sphere hydrogen-bonding network that varies with the state of protonation of the phosphonate moiety. Upon protonation of the complex, the second-sphere hydration probably becomes more ordered, which may result in a decrease in penetrability and an increase in tauM. The relaxivity of the Gd(III) complex is almost independent of the pH and is equal to 4.7 s(-1) mM(-1) (20 MHz, pH 7 and 37 degrees C). The solid

SPECTROSCOPIC STUDIES OF SOME LANTHANIDE(III) NITRATE ...

African Journals Online (AJOL)

a

The first method involves condensation of keto precursors with polyamines by the template method [11, 12] and in the second method, the ligand is first synthesized and isolated and the metal ion added to prepare the complexes [13, 14]. In our previous research on transition metal complexes we have used both routes ...

Extended lanthanide-transition metal arrays with cyanide bridges: syntheses, structures, and catalytic applications

International Nuclear Information System (INIS)

Liu Shengming; Poplaukhin, Pavel; Ding Errun; Plecnik, Christine E.; Chen Xuenian; Keane, Mark A.; Shore, Sheldon G.

2006-01-01

Systematic synthetic procedures produced several different structural types of extended lanthanide-transition metal (group 10) complexes with cyanide bridges. Of these, one-dimensional ladder arrays containing a Yb-Pd combination have been converted to bimetallic heterogeneous catalysts on an oxide (SiO 2 ) surface that is more effective than supported Pd alone. Two lanthanide-Cu(I) complexes have been prepared. One type, an inclusion complex consists of lanthanide(III) cations encapsulated in the pockets of a three-dimensional anionic array that contains Cu(I)-CN-Cu(I) bridges. The second type, an extended layer complex, consists of joined five-membered rings in a 'tile-like' pattern with Ln-CN-Cu and Cu-CN-Cu bridges

Syntheses of copper complexes of nicotinohydroxamic and ...

African Journals Online (AJOL)

Nicotinohydroxamic acid (NHA) and isonicotinohydroxamic acid (INHA) were synthesized, characterized by electronic and spectral studies,magnetic measurements and their pKa determined spectrophotometrically as 8.68 ± 0.02 in aqueous medium of 0.1mol dm-3 I=ionic strength. The composition of the complexes was ...

Syntheses, structures, and photoluminescence of lanthanide coordination polymers based on 4-oxo-1,4-dihydro-2,6-pyridinedicarboxylic acid

Energy Technology Data Exchange (ETDEWEB)

Qian, Jing; Li, Lei; Peng, Jing-Wei; Qiao, Wei-Wei; Sun, Mei-Mei [College of Chemistry, Tianjin Normal University, Tianjin (China); Gu, Wen [College of Chemistry, Nankai University, Tianjin (China)

2018-03-15

Investigating the coordination chemistry of H{sub 2}CDA (4-oxo-1,4-dihydro-2,6-pyridinedicarboxylic acid) with rare earth salts Ln(NO{sub 3}){sub 3} under hydrothermal conditions, structure transformation phenomenon was observed. The ligand, H{sub 2}CDA charged to its position isomer, enol type structure, H{sub 3}CAM (4-hydroxypyridine-2,6-dicarboxylic acid). Six new lanthanide(III) coordination polymers with the formulas [Ln(CAM)(H{sub 2}O){sub 3}]{sub n} [Ln = La (1), Pr, (2)] and {[Ln(CAM)(H_2O)_3].H_2O}{sub n} [Ln = Nd, (3), Sm, (4), Eu, (5), Y, (6)] were synthesized and characterized. The X-ray structure analyses show two kinds of coordination structures. The complexes 1 and 2 and 3-6 are isostructural. Complexes 1 and 2 crystallize in the monoclinic C{sub 2}/c space group, whereas 3-6 crystallize in the monoclinic system with space group P2{sub 1}/n. In the two kinds of structures, H{sub 3}CAM displays two different coordination modes. The Sm{sup III} and Eu{sup III} complexes exhibit the corresponding characteristic luminescence in the visible region at an excitation of 376 nm. (copyright 2018 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

cis-Aquabis(2,2′-bipyridine-κ2N,N′fluoridochromium(III bis(perchlorate dihydrate

Directory of Open Access Journals (Sweden)

Torben Birk

2010-02-01

Full Text Available The title mixed aqua–fluoride complex, [CrF(C10H8N22(H2O](ClO42·2H2O, has been synthesized by aquation of the corresponding difluoride complex using lanthanide(III ions as F− acceptors. The complex crystallizes with a CrIII ion at the center of a distorted octahedral coordination polyhedron with a cis arrangement of ligands. The crystal packing shows a hydrogen-bonding pattern involving water molecules, the coordinated F atom and the perchlorate anions

Fixation of carbon dioxide by macrocyclic lanthanide(III) complexes under neutral conditions producing self-assembled trimeric carbonato-bridged compounds with μ3-η2:η2:η2 bonding.

Science.gov (United States)

Bag, Pradip; Dutta, Supriya; Biswas, Papu; Maji, Swarup Kumar; Flörke, Ulrich; Nag, Kamalaksha

2012-03-28

A series of mononuclear lanthanide(III) complexes [Ln(LH(2))(H(2)O)(3)Cl](ClO(4))(2) (Ln = La, Nd, Sm, Eu, Gd, Tb, Lu) of the tetraiminodiphenolate macrocyclic ligand (LH(2)) in 95 : 5 (v/v) methanol-water solution fix atmospheric carbon dioxide to produce the carbonato-bridged trinuclear complexes [{Ln(LH(2))(H(2)O)Cl}(3)(μ(3)-CO(3))](ClO(4))(4)·nH(2)O. Under similar conditions, the mononuclear Y(III) complex forms the dimeric compound [{Y(LH(2))(H(2)O)Cl}(μ(2)-CO(3)){Y(LH(2))(H(2)O)(2)}](ClO(4))(3)·4H(2)O. These complexes have been characterized by their IR and NMR ((1)H, (13)C) spectra. The X-ray crystal structures have been determined for the trinuclear carbonato-bridged compounds of Nd(III), Gd(III) and Tb(III) and the dinuclear compound of Y(III). In all cases, each of the metal centers are 8-coordinate involving two imine nitrogens and two phenolate oxygens of the macrocyclic ligand (LH(2)) whose two other imines are protonated and intramolecularly hydrogen-bonded with the phenolate oxygens. The oxygen atoms of the carbonate anion in the trinuclear complexes are bonded to the metal ions in tris-bidentate μ(3)-η(2):η(2):η(2) fashion, while they are in bis-bidentate μ(2)-η(2):η(2) mode in the Y(III) complex. The magnetic properties of the Gd(III) complex have been studied over the temperature range 2 to 300 K and the magnetic susceptibility data indicate a very weak antiferromagnetic exchange interaction (J = -0.042 cm(-1)) between the Gd(III) centers (S = 7/2) in the metal triangle through the carbonate bridge. The luminescence spectral behaviors of the complexes of Sm(III), Eu(III), and Tb(III) have been studied. The ligand LH(2) acts as a sensitizer for the metal ions in an acetonitrile-toluene glassy matrix (at 77 K) and luminescence intensities of the complexes decrease in the order Eu(3+) > Sm(3+) > Tb(3+).

Investigation of formation constant of complex of a new synthesized ...

African Journals Online (AJOL)

The complex formation between a newly synthesized tripodal ligand and the cation Cu2+ in water and surfactant media was studied spectrophotometrically using rank annihilation factor analysis (RAFA). According to molar ratio data the stoichiometry of complexation between the ligand and the cation Cu2+ was 1:1.

cis-Aquabis(2,2'-bipyridine-κ2N,N')-fluoridochromium(III) bis(perchlorate) dihydrate

DEFF Research Database (Denmark)

Birk, Torben; Bendix, Jesper

2010-01-01

The title mixed aqua-fluoride complex, [CrF(C(10)H(8)N(2))(2)(H(2)O)](ClO(4))(2)·2H(2)O, has been synthesized by aqua-tion of the corresponding difluoride complex using lanthan-ide(III) ions as F(-) acceptors. The complex crystallizes with a Cr(III) ion at the center of a distorted octa-hedral co......-hedral coordination polyhedron with a cis arrangement of ligands. The crystal packing shows a hydrogen-bonding pattern involving water mol-ecules, the coordinated F atom and the perchlorate anions....

Synthesis and spectral studies of some lanthanide(III) complexes ...

African Journals Online (AJOL)

... compounds were characterized through various physico-chemical studies. The coordinating ligand DABAAPS behave as tridentate N,N,O-donors. The central metal ion displays the coordination number nine in these complexes. Thermal stabilities of these complexes were also studied through thermogravimetric analysis.

A combinatorial approach of inclusion complexation and dendrimer synthesization for effective targeting EGFR-TK.

Science.gov (United States)

Shende, Pravin; Patil, Sampada; Gaud, R S

2017-07-01

The aim of the present study was to use a combinatorial approach of inclusion complexation and dendrimer synthesization of gefitinib using solvent-free technique for targeting EGFR-TK to treat Non-Small-Cell Lung Cancer (NSCLC). The inclusion complex of gefitinib with β-cyclodextrin was prepared by trituration method. This complex encapsulated G4 PAMAM dendrimers were synthesized by Michael addition and amidation reactions using green chemistry and then PEGylated by conjugation reaction. FTIR and DSC confirmed the formation of inclusion complex of gefitinib and β-cyclodextrin and PEGylation of G4 PAMAM dendrimers. Gefitinib showed higher solubility, encapsulation efficiency and controlled release profile from PEGylated dendrimers compared to inclusion complex. The PEGylated dendrimers of inclusion complex of gefitinib were found to reduce hemolytic toxicity and lesser GI 50 value on Human lung cancer cell line A-549 by effective targeting EGFR-TK. A combinatorial approach of inclusion complexation and dendrimer synthesization is one of the alternative advanced approaches to treat NSCLC. Copyright © 2017 Elsevier B.V. All rights reserved.

Lanthanide(III) Complexes with Tridentate Schiff Base Ligand ...

African Journals Online (AJOL)

Lanthanide complexes, hydrazino, antioxidant activity, X-ray structure. 1. Introduction ... measured using a Johnson Matthey scientific magnetic suscepti- bility balance. 2.1. .... of the ligand and that the nitrogen atom supporting this proton is not involved in the ... 4f-electrons are not involved in the coordination. These facts.

Method for synthesizing metal bis(borano) hypophosphite complexes

Science.gov (United States)

Cordaro, Joseph G.

2013-06-18

The present invention describes the synthesis of a family of metal bis(borano) hypophosphite complexes. One procedure described in detail is the syntheses of complexes beginning from phosphorus trichloride and sodium borohydride. Temperature, solvent, concentration, and atmosphere are all critical to ensure product formation. In the case of sodium bis(borano) hypophosphite, hydrogen gas was evolved upon heating at temperatures above 150.degree. C. Included in this family of materials are the salts of the alkali metals Li, Na and K, and those of the alkaline earth metals Mg and Ca. Hydrogen storage materials are possible. In particular the lithium salt, Li[PH.sub.2(BH.sub.3).sub.2], theoretically would contain nearly 12 wt % hydrogen. Analytical data for product characterization and thermal properties are given.

Complexes of trivalent lanthanide ions with schiff base derived from vanillin and triethylenetetraamine

International Nuclear Information System (INIS)

Shahma, A.; Athar, M.; Ahmad, N.

1982-01-01

Complexes of lanthanide(III) ions with the schiff base derived from vanillin and triethylenetetraamine have been synthesised and characterised on the basis of elemental analyses, molar conductance, magnetic moment, IR and thermal analysis data. The thermograms show the elimination (OH)(OCH 3 )C 6 H 3 CH-group at low temperatures before the elimination of triethylenetetraamine part corroborating the observation made on the basis of IR spectral data. This is a clear indication of the non-coordination of the phenolic hydroxyl groups. The lanthanide ions in the complexes exhibit eight coordination numbers. (author)

A Physicochemical and Pharmacological Study of the Newly Synthesized Complex of Albendazole and the Polysaccharide Arabinogalactan from Larch Wood.

Science.gov (United States)

Chistyachenko, Yulia S; Meteleva, Elizaveta S; Pakharukova, Maria Y; Katokhin, Aleksey V; Khvostov, Mikhail V; Varlamova, Anastasiya I; Glamazdin, Igor I; Khalikov, Salavat S; Polyakov, Nikolay E; Arkhipov, Ivan A; Tolstikova, Tatyana G; Mordvinov, Viatcheslav A; Dushkin, Alexander V; Lyakhov, Nikolay Z

2015-01-01

Inclusion complexes of albendazole (ABZ) with the polysaccharide arabinogalactan from larch wood Larix sibirica and Larix gmelinii were synthesized using a solid-state mechanochemical technology. We investigated physicochemical properties of the synthesized complexes in the solid state and in aqueous solutions as well as their anthelmintic activity against Trichinella spiralis, Hymenolepis nаna, Fasciola hepatica, Opisthorchis felineus, and mixed nematodoses of sheep. Formation of the complexes was demonstrated by means of intrinsic solubility and the NMR relaxation method. The mechanochemically synthesized complexes were more stable in comparison with the complex produced by mixing solutions of the components. The complexes of ABZ showed anthelmintic activity at 10-fold lower doses than did free ABZ. The complexes also showed lower acute toxicity and hepatotoxicity. These results suggest that it is possible to design new drugs on the basis of the ABZ:arabinogalactan complex that are safer and more effective than albendazole.

Aryldiazo complexes. Syntheses and reactions of new complexes of osmium and ruthenium

International Nuclear Information System (INIS)

Haymore, B.L.; Ibers, J.A.

1975-01-01

Aryldiazo complexes, [M(CO) 2 (NNPh)(PPh 3 ) 2 ][PF 6 ](M = Os, Ru; Ph = C 6 H 5 ), were prepared by allowing diazonium salts to react with M(CO) 3 (PPh 3 ) 2 . Infrared spectra of the Ru complex suggest the presence of two isomers both in solution and in the solid state. These complexes react with a variety of coordinating anions (X - ), to form MX(CO) 2 (NNPh)(PPh 3 ) 2 . The osmium derivatives have ν(NN) near 1455 cm -1 , which is the lowest value yet reported for a nonbridging aryldiazo ligand. The first aryldiazo--hydrido complexes, MH(CO) 2 (NNPh)(PPh 3 ) 2 and MH(CO)(NNPh)(PPh 3 ) 2 , were prepared by deprotonation of the respective phenyldiazene complexes, MH(CO) 2 (HNNPh)(PPh 3 ) 2 + and MH(CO)(HNNPh)(PPh 3 ) 3 + . The compound OsCl 3 (NNPh)(PPh 3 ) 2 was also prepared. A large number of the foregoing complexes were synthesized with selective 2 H and 15 N labels. Infrared and NMR spectra show MX(CO) 2 (NNPh)(PPh 3 ) 2 and the analogous hydrido complex to be pseudooctahedral with trans phosphine ligands, cis carbonyl ligands, and a doubly bent phenyldiazenido (NNPh - ) ligand. Similarly, MH(CO)(NNPh)(PPh 3 ) 2 possesses a trigonal-bipyramidal geometry with trans phosphine ligands and an equatorial, singly bent phenyldiazoniumato (NNPh + ) ligand. Isotopic substitution of the diazo ligand shows that ν(NN) is often vibrationally coupled with phenyl vibrational modes and that two or three bands sometimes shift upon 15 N substitution. Vibrational coupling was also observed in the higher energy region (1850 to 1900 cm -1 ) in the compound RuCl 3 (NNC 6 D 5 )(PPh 3 ) 2 . The wide range in the values of ν(NN), RuCl 3 (NNPh)(PPh 3 ) 2 (1882 cm -1 ) vs. RuCl(CO) 2 (NNPh)(PPh 3 ) 2 (1462 cm -1 ), indicates that the N--N stretching frequencies are sensitive to the electronic and steric environment of the diazo ligand. The aryldiazo complexes are compared with analogous, isoelectronic nitrosyl complexes of Os and Ru

Design and Syntheses of Novel Fluoroporphyrin-Anthraquinone Complexes as Antitumor Agents.

Science.gov (United States)

Yang, Gu-Liang; Zhao, Sheng-Fang; Chen, Nian-You; Li, Shiming

2016-01-01

A novel fluoroporphyrin-anthraquinone hybrid with dipeptide link and its metal complexes were synthesized and evaluated for anti-proliferation activity in human cancer cell line HeLa. The preliminary results demonstrated that all the compounds showed moderate to excellent antitumor activities. Among the active compounds, compound 3 which contains fluorinated porphyrin-anthraquinone and zinc ion exhibited the highest potency with IC50 value of 8.83 µM, indicating that it was a promising antitumor candidate.

Lanthanide(III) complexes of bis-semicarbazone and bis-imine-substituted phenanthroline ligands: solid-state structures, photophysical properties, and anion sensing.

Science.gov (United States)

Nadella, Sandeep; Selvakumar, Paulraj M; Suresh, Eringathodi; Subramanian, Palani S; Albrecht, Markus; Giese, Michael; Fröhlich, Roland

2012-12-21

Phenanthroline-based hexadentate ligands L(1) and L(2) bearing two achiral semicarbazone or two chiral imine moieties as well as the respective mononuclear complexes incorporating various lanthanide ions, such as La(III), Eu(III), Tb(III), Lu(III), and Y(III) metal ions, were synthesized, and the crystal structures of [ML(1)Cl(3)] (M=La(III), Eu(III), Tb(III), Lu(III), or Y(III)) complexes were determined. Solvent or water molecules act as coligands for the rare-earth metals in addition to halide anions. The big Ln(III) ion exhibits a coordination number (CN) of 10, whereas the corresponding Eu(III), Tb(III), Lu(III), and Y(III) centers with smaller ionic radii show CN=9. Complexes of L(2), namely [ML(2)Cl(3)] (M=Eu(III), Tb(III), Lu(III), or Y(III)) ions could also be prepared. Only the complex of Eu(III) showed red luminescence, whereas all the others were nonluminescent. The emission properties of the Eu derivative can be applied as a photophysical signal for sensing various anions. The addition of phosphate anions leads to a unique change in the luminescence behavior. As a case study, the quenching behavior of adenosine-5'-triphosphate (ATP) was investigated at physiological pH value in an aqueous solvent. A specificity of the sensor for ATP relative to adenosine-5'-diphosphate (ADP) and adenosine-5'-monophosphate (AMP) was found. (31)P NMR spectroscopic studies revealed the formation of a [EuL(2)(ATP)] coordination species. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Syntheses and structures of technetium(V) and rhenium(V) oxo complexes of peptide having KYC-sequence

International Nuclear Information System (INIS)

Takayama, T.; Suzuki, K.; Sekine, T.; Kudo, H.

2000-01-01

Technetium(V) and rhenium(V) oxo complexes of a peptide having a KYC-sequence such as KYCAR (H 3 L 5 ) and KYCAREPPTRTNAYQGQG-NH 2 (H 3 L 18 ) were synthesized, and structures of the complexes were characterized by spectroscopic techniques. All of the complexes were synthesized by the ligand exchange reaction of [(n-C 4 H 9 ) 4 N][MOCl 4 ] (M = 99 Tc, Re) with peptide in methanol or dimethylformamide solution. These complexes have a square pyramidal structure with an oxo ligand at the apical position. The peptide is coordinated to a metal atom through N amine of lysine. S thiol of cysteine, and N amide of tyrosine and cysteine in the equatorial plane. A lysine (CH 2 ) 4 NH 2 group of the L 5 ligand has the syn conformation with respect to metal-oxo bonding in the complex. The syn isomer was selectively formed in the ligand exchange reaction. The conversion of the syn isomer to the anti isomer was observed only for syn-[ReO(L 5 )], in which the coordination of water to the trans position of the oxo ligand was involved. (orig.)

Syntheses and Characterization of Some Tetradentate Schiff-Base Complexes and Their Heteroleptic Analogues

Directory of Open Access Journals (Sweden)

A. A. Osowole

2008-01-01

Full Text Available VO(IV, Ni(II and Cu(II complexes of the asymmetric Schiff base [(HOC6H3(OCH3C(C6H5:N(CH2CH2N:C(CH3CH:C(C6H5OH], and their heteroleptic analogues with triphenyl phosphine and 2,2’-bipyridine have been synthesized and characterized by elemental analyses, conductance, magnetic, infrared and electronic spectral measurements. The ligand is tetradentate coordinating via the imine N and enolic O atoms. The Ni(II and Cu(II complexes adopt a four coordinate square planar geometry, the VO(IV complex is five coordinate square-pyramidal and the heteroleptic complexes are 6-coordinate, octahedral. The assignment of geometry is collaborated by magnetic moments and electronic spectra measurements. The compounds are non-electrolyte in nitromethane and are magnetically dilute.

Syntheses and structures of technetium(V) and rhenium(V) oxo complexes of peptide having KYC-sequence

Energy Technology Data Exchange (ETDEWEB)

Takayama, T.; Suzuki, K.; Sekine, T.; Kudo, H. [Dept. of Chemistry, Tohoku Univ., Sendai (Japan)

2000-07-01

Technetium(V) and rhenium(V) oxo complexes of a peptide having a KYC-sequence such as KYCAR (H{sub 3}L{sup 5}) and KYCAREPPTRTNAYQGQG-NH{sub 2} (H{sub 3}L{sup 18}) were synthesized, and structures of the complexes were characterized by spectroscopic techniques. All of the complexes were synthesized by the ligand exchange reaction of [(n-C{sub 4}H{sub 9}){sub 4}N][MOCl{sub 4}] (M = {sup 99}Tc, Re) with peptide in methanol or dimethylformamide solution. These complexes have a square pyramidal structure with an oxo ligand at the apical position. The peptide is coordinated to a metal atom through N{sub amine} of lysine. S{sub thiol} of cysteine, and N{sub amide} of tyrosine and cysteine in the equatorial plane. A lysine (CH{sub 2}){sub 4}NH{sub 2} group of the L{sup 5} ligand has the syn conformation with respect to metal-oxo bonding in the complex. The syn isomer was selectively formed in the ligand exchange reaction. The conversion of the syn isomer to the anti isomer was observed only for syn-[ReO(L{sup 5})], in which the coordination of water to the trans position of the oxo ligand was involved. (orig.)

Studies on mixed ligand complexes of lanthanide (III) ions

International Nuclear Information System (INIS)

Rajendran, G.; Usha Devi, K.G.

2002-01-01

As part of our research programme, we have prepared and characterized a few nitrato, thiocyanato and perchlorato complexes of lanthanide(III) ions with ligands, viz., a Schiff base derived from p-anisidine and vanillin and diphenyl sulphoxide. The complexes were characterized by the measurement of electrical conductances and magnetic susceptibilities, molecular mass and metal percentage and spectral analysis. The thermal decompositions were studied by TG and DTG techniques. The thiocyanato complexes were prepared by substitution method from nitrato complexes. p-Anisidine-vanillin (HDDA) and diphenyl sulphoxide (DPSO) are coordinated to the metal ion in unidentate fashion. All the anions were involved in coordination in these complexes. Thus they were found to have non- electrolytic behaviour with composition [Ln(HDDA) 2 (DPSO)X 3 ] where X = NO 3 ) or SCN perchlorato complexes were prepared from metal perchlorate as done in the case of nitrato complexes. They were found to have electrical conductance which corresponds to 1 : 1 electrolyte. Hence one of the perchlorate ions is outside the coordination sphere. The composition of this complex is found to be [Ln(HDDA) 3 (DPSO)(ClO 4 ) 2 ]ClO 4 . (author)

A role of copper(II) ions in the enhancement of visible and near-infrared lanthanide(III) luminescence

International Nuclear Information System (INIS)

Eliseeva, Svetlana V.; Golovach, Iurii P.; Liasotskyi, Valerii S.; Antonovich, Valery P.; Petoud, Stéphane; Meshkova, Svetlana B.

2016-01-01

Most of the existing optical methods for Cu II detection rely on a “turn-off” approach using visible lanthanide(III) luminescence. In this work we present an innovative molecular systems where the podands bis(2-hydrazinocarbonylphenyl) ethers of ethylene glycol (L1) and diethylene glycol (L2) have been designed, synthesised and tested with an ultimate goal to create a "turn-on" lanthanide(III)-based molecular probe for the specific detection of Cu II ions based on both visible (Tb III , Eu III ) and near-infrared (Nd III , Yb III ) emission. Quantum yields of the characteristic Ln III emission signals increases by at least two-orders of magnitude upon addition of Cu II into water/acetonitrile (9/1) solutions of LnL (L=L1, L2) complexes. A detailed investigation of ligand-centred photophysical properties of water/acetonitrile (9/1) solutions of CuL, GdL and GdCuL complexes revealed that the presence of Cu II ions does not significantly affect the energy positions of the singlet (32,260 cm −1 ) and triplet (25,640–25,970 cm −1 ) states, but partially or fully eliminates the singlet state quenching through an electron transfer mechanism. This effect increases the probability of intersystem crossing leading to enhanced triplet-to-singlet emission ratio and to longer triplet state lifetimes. The redox activity of hydrazine moieties and their ability to reduce Cu II to Cu I has been indicated by a qualitative assay with neocuproine. Finally, the probe demonstrates a good selectivity towards Cu II over other transition metal ions: the addition of divalent Zn II , Cd II , Pd II , Ni II , Co II or trivalent Fe III , Ga III , In III ion salts into solutions of TbL either does not affect emission intensity or increases it to a maximum of 2–3 times, while, under similar experimental conditions, the presence of Cu II results in a 20- to 30-times lanthanide luminescence enhancement. This new strategy results in a versatile and selective optical platform for the

Prism inside. Spectroscopic and magnetic properties of the lanthanide(III) chloride oxidotungstates(VI) Ln{sub 3}Cl{sub 3}[WO{sub 6}] (Ln = La - Nd, Sm - Tb)

Energy Technology Data Exchange (ETDEWEB)

Dorn, Katharina V.; Blaschkowski, Bjoern; Hartenbach, Ingo [Institute for Inorganic Chemistry, University of Stuttgart (Germany); Foerg, Katharina; Netzsch, Philip; Hoeppe, Henning A. [Institute for Physics, University of Augsburg (Germany)

2017-11-17

The lanthanide(III) chloride oxidotungstates(VI) with the formula Ln{sub 3}Cl{sub 3}[WO{sub 6}] for Ln = La - Nd, Sm - Tb were synthesized by solid-state reactions utilizing the respective lanthanide trichloride, lanthanide sesquioxide (where available), and tungsten trioxide together with lithium chloride as flux. The title compounds crystallize hexagonally in space group P6{sub 3}/m (no. 176, a = 941-909, c = 543-525 pm, Z = 2). The structures comprise crystallographically unique Ln{sup 3+} cations surrounded by six O{sup 2-} and four Cl{sup -} anions (C.N. = 10) forming distorted tetracapped trigonal prisms as well as rather uncommon trigonal prismatic [WO{sub 6}]{sup 6-} units, whose edges are coordinated by nine Ln{sup 3+} cations. Thus, a {sup 3}{sub ∞}{([WO_6]Ln"e_9_/_3)"3"+} framework (e = edge-sharing) is created, which contains tube-shaped channels along [001] lined with chloride anions. To elucidate the spectroscopic and magnetic properties of the obtained pure phase samples, single-crystal Raman (for Ln = La - Nd, Sm-Tb), diffuse reflectance (for Ln = La, Pr, Nd, Gd), and luminescence spectroscopy (for bulk Ln{sub 3}Cl{sub 3}[WO{sub 6}] (Ln = La, Eu, Gd, Tb) and Eu{sup 3+}- or Tb{sup 3+}-doped derivatives of La{sub 3}Cl{sub 3}[WO{sub 6}] and Gd{sub 3}Cl{sub 3}[WO{sub 6}], respectively) were performed and their temperature-dependent magnetic moments (for Ln = Pr, Nd, Gd) were determined. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Synthesis, characterization and anticancer activities of two lanthanide(III) complexes with a nicotinohydrazone ligand

Science.gov (United States)

Xu, Zhou-Qin; Mao, Xian-Jie; Jia, Lei; Xu, Jun; Zhu, Tao-Feng; Cai, Hong-Xin; Bie, Hong-Yan; Chen, Ru-Hua; Ma, Tie-liang

2015-12-01

Two isostructural acylhydrazone based complexes, namely [Ce(penh)2(H2O)4](NO3)3·4H2O (1) and [Sm(penh)2(NO3)2](NO3)·C2H5OH (2) (penh = 2-acetylpyridine nicotinohydrazone), have been obtained and characterized by physico-chemical and spectroscopic methods. The ten-coordinated lanthanide metal ion in each complex is surrounded by two independent tridentate neutral acylhydrazones with two ON2 donor sets. The other four coordination oxygen atoms are from four water molecules and two bidentate nitrate anions for complexes 1 and 2, respectively, thus giving distorted bicapped square antiprism geometry. Both complexes have excellent antitumor activity towards human pancreatic cancer (PATU8988), human colorectal cancer (lovo) and human gastric cancer(SGC7901) cell line. Furthermore, the cell apoptosis of complex 1 is detected by AnnexinV/PI flow cytometry.

Electro-spray Ionization Mass Spectrometry Investigation of BTBP - Lanthanide(III) and Actinide(III) Complexes

Energy Technology Data Exchange (ETDEWEB)

Retegan, T.; Ekberg, Ch. [Chalmers, Dept Chem and Biol Engn, SE-41296 Gothenburg, (Sweden); Berthon, L.; Zorz, N. [DEN DRCP SCPS LCSE, CEA Marcoule, Bagnols Sur Ceze, (France)

2009-07-01

In the framework of nuclear waste reprocessing, the separation processes of minor actinides from fission products are developed using liquid-liquid extraction. To gain an understanding of the mechanism involved in the extraction process, a complex formation of actinides and lanthanides with BTBPs (6, 6'-bis(5, 6-dialkyl-1, 2, 4-triazin-3-yl)-2, 2'-bipyridines) was characterized using the Electro-spray Ionization Mass Spectrometry (ESI-MS) technique. This study was carried out to compare the influence of diluents and side groups of the extractants on complex formation. Three different diluents, nitrobenzene, octanol and cyclohexanone, and two extractants, C5-BTBP and CyMe{sub 4}-BTBP, were selected for this experiment. It was found that the change of the diluent and of the substituent on the BTBP moiety does not modify the stoichiometry of the complexes which is L{sub 2}M(NO{sub 3}){sub 3}. It is proposed that one nitrate is directly coordinated to the metal ion, the two other anions probably remaining in the outer coordination sphere. The difference observed in extracting properties is probably due to the solvation of the complexes by the diluent. The noncovalent force that holds complexes together are likely to be largely governed by electrostatic interactions even if the hydrophobic exterior of the complexes plays an important role in the complexation/extraction mechanism. The study of the stability of the ions in the gas phase shows that the C5-BTBP ligand has a labile hydrogen atom, which is a fragility point of C5-BTBP. (authors)

Thermal and biological evolution of Fe(III)-Sulfanilamide complexes synthesized by green strategy

Science.gov (United States)

Prajapat, Garima; Rathore, Uma; Gupta, Rama; Bhojak, N.

2018-05-01

Sulfonamides belong to a category of sulfadrugs, that are widely used as antibiotic medicines. Their metal complexes, also called Metallodrugs, are known to have diverse pharmacological applications and are significantly used as therapeutic agents for treatment of several human diseases. Fe(III) complexes of two sulfonamides, namely Sulfanilamide and Sulfadiazine have been synthesized by the method of Microwave Assisted Organic Synthesis (MAOS), using acetone as solvent medium. Presence of excellent donor atoms such as N and O, induce these drugs to exhibit a chelating behavior with the metal ion, and to act as bidentate ligands. Both the complexes were found to have four coordinated, tetrahedral geometry with one molecule of water of crystallisation. Thermal decomposition studies were carried out in an inert nitrogen atmosphere by Thermogravimetric (TGA) and Derivative Thermogravimetric (DTA) analysis. Interpretation of thermograms have been done to evaluate various kinetic and thermodynamic parameters, using integral method of Coats and Redfern. The antibacterial activity for both complexes have been screened against E.coli, S. aureus and B. subtilis.

New lanthanide(III) complexes of chiral nonadendate macrocyclic amine derived from (1R,2R)-1,2-diaminocyclohexane and 2,6-diformyl-4-methylphenol

Energy Technology Data Exchange (ETDEWEB)

Paluch, Marta [Department of Chemistry, University of Wroclaw, 14 F. Joliot-Curie, 50-383 Wroclaw (Poland); Lisowski, Jerzy [Department of Chemistry, University of Wroclaw, 14 F. Joliot-Curie, 50-383 Wroclaw (Poland)], E-mail: jurekl@wchuwr.chem.uni.wroc.pl

2008-02-28

The series of complexes [LnH{sub 4}L(NO{sub 3}){sub 2}](NO{sub 3}){sub 2}.nH{sub 2}O (Ln = La, Ce, Pr, Nd, Gd, Tb, Ho, Er, Tm) of the positively charged protonated form of a chiral macrocyclic amine H{sub 4}L{sup +}, derived from the 3 + 3 condensation product of (1R,2R)-1,2-diaminocyclohexane and 2,6-diformyl-4-methylphenol, have been synthesized. The series of complexes Na{sub x}[LnL](X){sub y}(OH){sub x-y}.n(solv) (X = NO{sup 3-} or Cl{sup -}, and Ln = La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) of the deprotonated anionic form of the ligand, L{sup 3-}, have also been synthesised. The complexes have been characterised by elemental analyses, {sup 1}H NMR and ESI MS spectra. The X-ray crystal structures of the [LaH{sub 4}L(NO{sub 3}){sub 2}](NO{sub 3}){sub 2}.5CH{sub 3}OH and [GdH{sub 4}L(NO{sub 3}){sub 2}](NO{sub 3}){sub 2}.5CH{sub 3}OH complexes have been determined. The two complexes are isostructural, and the protonated macrocycle acts as pentadentate ligand. The Ln(III) ion is bound to three phenolate oxygen atoms and two amine nitrogen atoms of the macrocyclic ligand and its coordination sphere is completed by the two axial bidendate nitrate anions.

Complexes cobalt(II, zinc(II and copper(II with some newly synthesized benzimidazole derivatives and their antibacterial activity

Directory of Open Access Journals (Sweden)

S. O. PODUNAVAC-KUZMANOVIC

1999-05-01

Full Text Available The preparation and properties of some complexes of cobalt(II, zinc(II and copper(II with several newly synthesized benzimidazole derivatives (L are reported. The complexes, of the general formula [MCl2L2] (M=Co(II, Zn(II and [CuCl2L(H2O], have a tetrahedral structure. The complexes were characterized by elemental analysis, molar conductivity, magnetic susceptibility measurements, IR and absorption electronic spectra. The antibacterial activitiy of the benzimidazoles and their complexes was evaluated against Erwinia carotovora subsp. carotovora and Erwinia amylovora. The complexes were found to be more toxic than the ligands.

A role of copper(II) ions in the enhancement of visible and near-infrared lanthanide(III) luminescence

Energy Technology Data Exchange (ETDEWEB)

Eliseeva, Svetlana V., E-mail: svetlana.eliseeva@cnrs-orleans.fr [Centre de Biophysique Moléculaire CNRS UPR 4301, Rue Charles Sadron, 45071 Orléans Cedex 2 (France); Le Studium, Loire Valley Institute for Advanced Studies, 1 Rue Dupanloup, 45000 Orléans (France); Golovach, Iurii P.; Liasotskyi, Valerii S. [I.I.Mechnikov Odessa National University, 2 Dvoryanska street, 65082 Odessa (Ukraine); Antonovich, Valery P. [A.V. Bogatsky Physico-Chemical Institute of the National Academy of Sciences of Ukraine, 86 Lustdorfskaya doroga, 65080 Odessa (Ukraine); Petoud, Stéphane, E-mail: stephane.petoud@inserm.fr [Centre de Biophysique Moléculaire CNRS UPR 4301, Rue Charles Sadron, 45071 Orléans Cedex 2 (France); Meshkova, Svetlana B., E-mail: s_meshkova@ukr.net [A.V. Bogatsky Physico-Chemical Institute of the National Academy of Sciences of Ukraine, 86 Lustdorfskaya doroga, 65080 Odessa (Ukraine)

2016-03-15

Most of the existing optical methods for Cu{sup II} detection rely on a “turn-off” approach using visible lanthanide(III) luminescence. In this work we present an innovative molecular systems where the podands bis(2-hydrazinocarbonylphenyl) ethers of ethylene glycol (L1) and diethylene glycol (L2) have been designed, synthesised and tested with an ultimate goal to create a 'turn-on' lanthanide(III)-based molecular probe for the specific detection of Cu{sup II} ions based on both visible (Tb{sup III}, Eu{sup III}) and near-infrared (Nd{sup III}, Yb{sup III}) emission. Quantum yields of the characteristic Ln{sup III} emission signals increases by at least two-orders of magnitude upon addition of Cu{sup II} into water/acetonitrile (9/1) solutions of LnL (L=L1, L2) complexes. A detailed investigation of ligand-centred photophysical properties of water/acetonitrile (9/1) solutions of CuL, GdL and GdCuL complexes revealed that the presence of Cu{sup II} ions does not significantly affect the energy positions of the singlet (32,260 cm{sup −1}) and triplet (25,640–25,970 cm{sup −1}) states, but partially or fully eliminates the singlet state quenching through an electron transfer mechanism. This effect increases the probability of intersystem crossing leading to enhanced triplet-to-singlet emission ratio and to longer triplet state lifetimes. The redox activity of hydrazine moieties and their ability to reduce Cu{sup II} to Cu{sup I} has been indicated by a qualitative assay with neocuproine. Finally, the probe demonstrates a good selectivity towards Cu{sup II} over other transition metal ions: the addition of divalent Zn{sup II}, Cd{sup II}, Pd{sup II}, Ni{sup II}, Co{sup II} or trivalent Fe{sup III}, Ga{sup III}, In{sup III} ion salts into solutions of TbL either does not affect emission intensity or increases it to a maximum of 2–3 times, while, under similar experimental conditions, the presence of Cu{sup II} results in a 20- to 30-times

Spectroscopic and structural study of the newly synthesized heteroligand complex of copper with creatinine and urea.

Science.gov (United States)

Gangopadhyay, Debraj; Singh, Sachin Kumar; Sharma, Poornima; Mishra, Hirdyesh; Unnikrishnan, V K; Singh, Bachcha; Singh, Ranjan K

2016-02-05

Study of copper complex of creatinine and urea is very important in life science and medicine. In this paper, spectroscopic and structural study of a newly synthesized heteroligand complex of copper with creatinine and urea has been discussed. Structural studies have been carried out using DFT calculations and spectroscopic analyses were carried out by FT-IR, Raman, UV-vis absorption and fluorescence techniques. The copper complex of creatinine and the heteroligand complex were found to have much increased water solubility as compared to pure creatinine. The analysis of FT-IR and Raman spectra helps to understand the coordination properties of the two ligands and to determine the probable structure of the heteroligand complex. The LIBS spectra of the heteroligand complex reveal that the complex is free from other metal impurities. UV-visible absorption spectra and the fluorescence emission spectra of the aqueous solution of Cu-Crn-urea heteroligand complex at different solute concentrations have been analyzed and the complex is found to be rigid and stable in its monomeric form at very low concentrations. Copyright © 2015 Elsevier B.V. All rights reserved.

Newly Synthesized Doxorubicin Complexes with Selected Metals—Synthesis, Structure and Anti-Breast Cancer Activity

Directory of Open Access Journals (Sweden)

Agata Jabłońska-Trypuć

2017-07-01

Full Text Available Doxorubicin (DOX is very effective chemotherapeutic agent, however it has several major drawbacks. Therefore the motivation for developing novel drug complexes as anticancer agents with different mechanism of action has arisen. The aim of the present study was to evaluate the influence of newly synthesized DOX complexes with selected metals (Mg, Mn, Co, Ni, Fe, Cu, Zn on apoptosis, cell cycle, viability, proliferation and cytotoxicity in the breast cancer cell line MCF-7. Complexation of DOX with metals has likewise been the subject of our research. The current work showed that the tested bivalent metals at a given pH condition formed metal:DOX complexes in a ratio of 2:1, while iron complexes with DOX in a ratio of 3:1. The studies also showed that selected metal-DOX complexes (Mg-DOX, Mn-DOX, Ni-DOX at 0.5 µM concentration significantly decreased cell viability and proliferation, however they increased caspase 7 activity. Results also indicated that studied metal-DOX complexes showed high cytotoxicity in MCF-7 cells. Therefore they were chosen for cell cycle check-points and apoptosis/necrosis analysis studied by flow cytometry. Obtained results suggest that doxorubicin complexed by specified metals can be considered as a potential anti-breast cancer agent, which is characterized by a higher efficacy than a parent drug.

Uranium hetero-bimetallic complexes: synthesis, structure and magnetic properties; Complexes heterobimetalliques de l'uranium: synthese, structure et proprietes magnetiques

Energy Technology Data Exchange (ETDEWEB)

Le Borgne, Th

2000-10-04

The aim of this thesis is to synthesize molecular complexes with uranium and transition metal ions in close proximity, to determine the nature of the magnetic interaction between them. We decided to use Schiff bases as assembling ligands, which are unusual for uranium (IV). Although the simplest Schiff bases, such as H{sub 2}Salen, lead to ligand exchange reactions, the bi-compartmental Schiff base H{sub 4}L{sup 6} (bis(3-hydroxy-salicylidene) - 2,2-dimethyl-propylene) allows the crystal structure determination of the complex [L{sup 6}Cu(pyr)]U[L{sup 6}Cu].2pyr, obtained by reaction of the metallo-ligand H{sub 2}L{sup 6}Cu with U(acac){sub 4}. In this manner, the complexes [L{sup 6}Co(pyr)]{sub 2}U and [L{sup 6}Ni(pyr)]{sub 2}U.pyr were also isolated, as well as the compounds in which the paramagnetic ions have been exchanged by the diamagnetic ions Zn{sup II}, Zr{sup IV} and Th{sup IV}': [L{sup 6}Zn(pyr)]{sub 2}U, [L{sup 6}Cu]{sub 2}Zr and [L{sup 6}Cu(pyr)]Th[L{sup 6}Cu].2pyr. These complexes are the first which involve three metallic centres assembling by the means of a hexa-dentate Schiff base. The crystalline structures show, for all these complexes, the outstanding orthogonal arrangement of the two fragments L{sup 6}M around the central atom which is in a dodecahedral environment of eight oxygen atoms of two Schiff bases. The syntheses of the isostructural complexes Cu2{sup II} and Zn{sub 2}U in which the uranium (IV) ion is close, in the first one, to the paramagnetic ion Cu{sup II} and, in the second one, to the diamagnetic ion Zn{sup II}, has allowed the use of the empiric method to determine the nature of the magnetic interaction between an f element and a transition metal. The comparison of the magnetic behaviour of two complexes Cu{sub 2}U and Zn{sub 2}U, expressed by the variation of {chi}T vs T, reveals the ferromagnetic interaction in the heart of the triad Cu-U-Cu. The magnetic behaviour of the complexes Cu{sub 2}Th et Cu{sub 2}Zr which does not

Syntheses, Crystal Structures and Thermal Behaviors of Two Supramolecular Salamo-Type Cobalt(II and Zinc(II Complexes

Directory of Open Access Journals (Sweden)

Gang Li

2017-07-01

Full Text Available This paper reports the syntheses of two new complexes, [Co(L1(H2O2] (1 and [{Zn(L2(μ-OAcZn(n-PrOH}2] (2, from asymmetric halogen-substituted Salamo-type ligands H2L1 and H3L2, respectively. Investigation of the crystal structure of complex 1 reveals that the complex includes one Co(II ion, one (L12− unit and two coordinated water molecules. Complex 1 shows slightly distorted octahedral coordination geometry, forming an infinite 2D supramolecular structure by intermolecular hydrogen bond and π–π stacking interactions. Complex 2 contains four Zn(IIions, two completely deprotonated (L23− moieties, two coordinated μ-OAc− ions and n-propanol molecules. The Zn(II ions in complex 2 display slightly distorted trigonal bipyramidal or square pyramidal geometries.

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African Journals Online (AJOL)

The values of the bonding parameter (b) and angular overlap parameter (m) were found to be positive indicating covalent bonding [21]. Table 3. Electronic spectral data (cm) and related bonding parameters of lanthanide(III) isothiocyanato complexes of DABAAPS. 80 . Complexes Ln(NCS). Complex Energy levels (1-B).

Three phenoxo-bridged dinuclear lanthanide complexes. Syntheses, crystal structures, and magnetic properties

Energy Technology Data Exchange (ETDEWEB)

Zhang, Zhi-Chao; Dai, Rui-Peng; Yang, En-Cui [College of Chemistry, Key Laboratory of Inorganic-Organic Hybrid Functional Material Chemistry, Tianjin Normal University (China); Dong, Hui-Ming; Zhao, Xiao-Jun [College of Chemistry, Key Laboratory of Inorganic-Organic Hybrid Functional Material Chemistry, Tianjin Normal University (China); Department of Chemistry, Collaborative Innovation Center of Chemical Science and Engineering, Nankai University, Tianjin (China)

2018-03-15

Three dinuclear lanthanide complexes [Ln{sub 2}(H{sub 2}L){sub 2}(NO{sub 3}){sub 4}] [Ln = Dy (1), Tb (2), and Gd (3)] [H{sub 3}L = 2-hydroxyimino-N'-[(2-hydroxy-3-methoxyphenyl)methylidene]- propanohydrazone] were solvothermally synthesized by varying differently anisotropic rare earth ions. Single-crystal structural analyses demonstrate that all the three complexes are crystallographically isostructural with two centrosymmetric Ln{sup III} ions aggregated by a pair of monodeprotonated H{sub 2}L{sup -} anions. Weak intramolecular antiferromagnetic interactions with different strength were mediated by a pair of phenoxo bridges due to superexchange and/or single-ion anisotropy. Additionally, the Dy{sup III}-based entity shows the strongest anisotropy exhibits field-induced single-molecule magnetic behavior with two thermally activated relaxation processes. In contrast, 3 with isotropic Gd{sup III} ion has a significant cryogenic magnetocaloric effect with the maximum entropy change of 25.7 J.kg{sup -1}.K{sup -1} at 2.0 K and 70.0 kOe. (copyright 2018 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Characterization of the lanthanum(III) and europium(III) trichloroacetate complexes extracted with 18-crown-6

International Nuclear Information System (INIS)

Imura, H.; Saito, Y.; Ohashi, K.; Meguro, Y.; Yoshida, Z.; Choppin, G.R.

1996-01-01

Extraction of lanthanide(III) ions with 18-crown-6 (18C6) and trichloroacetate (tca) has been studied. The composition, hydration, and structure of the La(III) and Eu(III) complexes extracted into 1,2-dichloroethane were investigated by using several methods such as the liquid-liquid distribution technique, conductimetry, Karl Fisher titration, laser luminescence spectroscopy, and 1 H NMR. The La(III) complex was found to be a monohydrate, La(tca) 3 (18C6)(H 2 O), while that of Eu(III) was a mixture of a monohydrate and a dihydrate, i.e., Eu(tca) 3 (18C6)(H 2 O) and Eu(tca) 3 (18C6)(H 2 O) 2 . The origin of the selectivity by 18C6 which gives much higher extractability of La(III) than of Eu(III) is explained by considering the hydration and probable structure of their complexes. 12 refs., 5 figs., 4 tabs

The influence of carboxilate, phosphinate and seleninate groups on luminescent properties of lanthanides complexes

International Nuclear Information System (INIS)

Monteiro, Jorge H.S.K.; Formiga, André L.B.; Sigoli, Fernando A.

2014-01-01

The lanthanides(III) complexes [Ln(bza) 3 (H 2 O) n ]·mH 2 O, [Ln(ppa) 3 (H 2 O) n ]·mH 2 O and [Ln(abse) 3 (H 2 O) n ]·mH 2 O where Ln=Eu 3+ , Gd 3+ or Tb 3+ were synthesized using sodium benzoate (Nabza), sodium phenylseleninate (Naabse) and sodium phenylphosphinate (Nappa) in order to verify the influence on coordination modes and the luminescence parameters when the carbon is exchanged by phosphorus or selenium in those ligands. The complexes' stoichiometries were determined by lanthanide(III) titration, microanalysis and TGA. The coordination modes were determined as bidentate bridging and chelate by the FT-IR. The triplet state energies of the ligands were obtained by two different approaches giving a difference of about ∼2000 cm −1 between them. The [Eu(abse) 3 (H 2 O)] complex shows the higher degree of covalence which was verified by the centroid of 5 D 0 → 7 F 0 transition (17,248 cm −1 ). On the other hand the [Ln(abse) 3 (H 2 O) n ]·mH 2 O complexes have an inefficient antenna effect verified by the low values of absolute emission quantum yields. The [Ln(ppa) 3 (H 2 O) n ]·mH 2 O complexes have higher emission decay lifetime values among the complexes which is a result of the ability of this ligand to form coordination polymers avoiding water molecules in the first coordination sphere. The [Eu(ppa) 3 ] complex has the highest point symmetry around europium(III) among the synthesized complexes, followed by the [Eu(bza) 3 (H 2 O) 2 ]·3/2(H 2 O) and [Eu(abse) 3 (H 2 O)] complexes where europium(III) show similar point symmetries. As one may expect, the triplet state energy position would change the transfer and/or back energy transfer rates from ligand to metal. The calculation of these rates show that the back energy transfer rates are more affected than the transfer ones by changing the triplet state energy in the range of ∼2000 cm −1 . The changes in the energy transfer rates from triplet state to europium(III) levels are not

Synthesis, X-ray crystal structure, DNA binding and Nuclease activity ...

Indian Academy of Sciences (India)

s12039-016-1125-x. Synthesis, X-ray crystal structure, DNA binding and Nuclease activity of lanthanide(III) complexes of 2-benzoylpyridine acetylhydrazone. KARREDDULA RAJA, AKKILI SUSEELAMMA and KATREDDI HUSSAIN REDDY. ∗.

EXAFS Phase Retrieval Solution Tracking for Complex Multi-Component System: Synthesized Topological Inverse Computation

International Nuclear Information System (INIS)

Lee, Jay Min; Yang, Dong-Seok; Bunker, Grant B

2013-01-01

Using the FEFF kernel A(k,r), we describe the inverse computation from χ(k)-data to g(r)-solution in terms of a singularity regularization method based on complete Bayesian statistics process. In this work, we topologically decompose the system-matched invariant projection operators into two distinct types, (A + AA + A) and (AA + AA + ), and achieved Synthesized Topological Inversion Computation (STIC), by employing a 12-operator-closed-loop emulator of the symplectic transformation. This leads to a numerically self-consistent solution as the optimal near-singular regularization parameters are sought, dramatically suppressing instability problems connected with finite precision arithmetic in ill-posed systems. By statistically correlating a pair of measured data, it was feasible to compute an optimal EXAFS phase retrieval solution expressed in terms of the complex-valued χ(k), and this approach was successfully used to determine the optimal g(r) for a complex multi-component system.

A [Cyclentetrakis(methylene)]tetrakis[2-hydroxybenzamide]Ligand That Complexes and Sensitizes Lanthanide(III) Ions

Energy Technology Data Exchange (ETDEWEB)

D' Aleo, Anthony; Xu, Jide; Do, King; Muller, Gilles; Raymond, Kenneth N.

2009-04-30

The synthesis of a cyclen derivative containing four isophthalamide groups (L{sup 1}) is described. The spectroscopic properties of the Ln(III) complexes of L{sup 1} (Ln = Gd, Tb, Yb, Eu) reveal changes of the UV/visible absorption, circular dichroism absorption, luminescence and circularly polarized luminescence properties. It is shown that at least two metal complex species are present in solution, whose relative amounts are pH dependent. When at pH > 8.0, an intense long lived emission is observed (for [L{sup 1}Tb] and [L{sup 1}Yb]) while at pH < 8.0, a weaker, shorter-lived species predominates. Unconventional Ln(III) emitters (Pr, Nd, Sm, Dy and Tm) were sensitized in basic solution, both in the visible and in the near infra-red, to measure the emission of these ions.

Synthesis and luminescent spectroscopy of lanthanide complexes with dimethylpyridine-2,6-dicarboxylate (dmpc)

Energy Technology Data Exchange (ETDEWEB)

Taha, Ziyad A., E-mail: tahaz33@just.edu.jo [Department of Applied Chemical Sciences, Faculty of Arts and Sciences, Jordan University of Science and Technology, Irbid 22110 (Jordan); Ajlouni, Abdulaziz M.; Hijazi, Ahmed K. [Department of Applied Chemical Sciences, Faculty of Arts and Sciences, Jordan University of Science and Technology, Irbid 22110 (Jordan); Al-Rawashdeh, Nathir A. [Department of Applied Chemical Sciences, Faculty of Arts and Sciences, Jordan University of Science and Technology, Irbid 22110 (Jordan); Department of Chemistry, United Arab Emirates University, Al Ain 15551 (United Arab Emirates); Al-Hassan, Khader A.; Al-Haj, Yaser A. [Department of Chemistry, Faculty of Science, Yarmouk University, 1163 Irbid (Jordan); Ebqa' ai, Mohammad A. [Al-Qunfudah Center For Scientific Research, Umm Al-Qura University, College in Al-Qunfudah, Makkah (Saudi Arabia); Altalafha, Ammar Y. [Department of Chemistry, Faculty of Science, Yarmouk University, 1163 Irbid (Jordan)

2015-05-15

A series of lanthanide complexes with the general formulae [Ln(dmpc)(NO{sub 3}){sub 2}(H{sub 2}O){sub 2}]NO{sub 3} (Ln=Pr, Nd, Sm, Eu, Gd, Tb, Dy, and Er) and [La(dmpc)(NO{sub 3}){sub 2}(H{sub 2}O){sub 2}]NO{sub 3} were prepared by direct reaction between hydrated lanthanide(III) nitrate and dimethylpyridine-2,6-dicarboxylate (dmpc) in a 1:1 M ratio in ethylacetate–chloroform mixture. The luminescence properties of the dmpc and its Ln(III) complexes were investigated in solid state and in methanol, DMF and DMSO solutions. The Tb–dmpc, Eu–dmpc, Sm–dmpc and Dy–dmpc complexes exhibit characteristic luminescence of Tb(III), Eu(III), Sm(III) and Dy(III) ions indicating energy transfer from the dmpc to the Ln(III) ions. Scavenging activities of the dmpc and its Ln(III) complexes on DPPH{sup •} free radical were investigated in DMSO solution at a different concentrations ranges. - Highlights: • Nine new lanthanide complexes with dmpc ligand are prepared and characterized. • Ln–dmpc {Ln=Eu, Tb, Sm, Dy} complexes exhibit characteristic emissions of Ln ions. • The solvent effect on the luminescence intensity is investigated. • The antioxidant activity of the dmpc is enhanced upon complexation with lanthanide.

Novel heterometallic metal–azido complex synthesized by “one-step” reaction: synthetic strategy and magnetic properties

International Nuclear Information System (INIS)

Jiao, Yong-Kun; Li, Xiu-Ping; Zhao, Cui; Wang, Hai-Chao; Xue, Min; Zhao, Jiong-Peng; Liu, Fu-Chen

2013-01-01

A novel heterometallic complex, [Ni 2 Mn(N 3 ) 2 (nic) 4 ·(H 2 O) 2 ] n (1) (nic=nicotinate), was obtained by assembling MnCl 2 ·4H 2 O, Ni(NO 3 ) 2 ·6H 2 O, NaN 3 and nicotinic acid with a “one step” synthetic strategy—hydrothermal reaction. The 3D structure of the complex can be described as end-on (EO) azido and syn,syn carboxylates mixed bridged by alternate Ni–Mn–Ni trimers linked by the nicotinate. Dominant ferromagnetic interactions were observed between the Ni II and Mn II ions in the trimer. - Graphical abstract: A novel heterometallic 3D complex [Ni 2 Mn(N 3 ) 2 (nic) 4 ·(H 2 O) 2 ] n (1) (nic=nicotinate) was synthesized by hydrothermal reaction. This complex exhibits interesting structural and magnetic properties. - Highlights: • It is difficult to construct simple coordination complexes with azide as “ligands” to obtain heterometallic metal–azido compounds. • A “one-step” method—hydrothermal reaction— was introduced to avoid the disadvantages of azide mentioned above. • The magnetic property is different with the isostructural homometal–azido complex due to the changed metal center

Copper(II) cyanido-bridged bimetallic nitroprusside-based complexes: Syntheses, X-ray structures, magnetic properties, 57Fe Moessbauer spectroscopy and thermal studies

International Nuclear Information System (INIS)

Travnicek, Zdenek; Herchel, Radovan; Mikulik, Jiri; Zboril, Radek

2010-01-01

Three heterobimetallic cyanido-bridged copper(II) nitroprusside-based complexes of the compositions [Cu(tet)Fe(CN) 5 NO].H 2 O (1), where tet=N,N'-bis(3-aminopropyl)ethylenediamine, [Cu(hto)Fe(CN) 5 NO].2H 2 O (2), where hto=1,3,6,9,11,14-hexaazatricyclo[12.2.1.1 6,9 ]octadecane and [Cu(nme) 2 Fe(CN) 5 NO].H 2 O (3), where nme=N-methylethylenediamine, were synthesized and characterized by elemental analyses, 57 Fe Moessbauer and FTIR spectroscopies, thermal analysis, magnetic measurements and single-crystal X-ray analysis. The products of thermal degradation processes of 2 and 3 were studied by XRD, 57 Fe Moessbauer spectroscopy, SEM and EDS, and they were identified as mixtures of CuFe 2 O 4 and CuO. - Three heterobimetallic cyano-bridged copper(II) nitroprusside-based complexes of the general compositions of [Cu(L)Fe(CN) 5 NO].xH 2 O, where L=N,N'-bis(3-aminopropyl)ethylenediamine (complex 1), 1,3,6,9,11,14-hexaazatricyclo[12.2.1.1 6,9 ]-octadecane (complex 2) and N-methylethylenediamine (complex 3), were synthesized, and fully structurally and magnetically characterized. SEM, EDS, XRD and 57 Fe Moessbauer experiments were used for characterization of thermal decomposition products of complexes 2 and 3.

Syntheses and luminescence properties of two novel lanthanide (III) perchlorate complexes with phenacyl p-tolyl sulfoxide

Energy Technology Data Exchange (ETDEWEB)

Feng, Shu-Yan [College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China); Li, Wen-Xian, E-mail: nmglwx@163.com [College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China); Zheng, Yu-Shan [Inner Mongolia Autonomous Region Product Quality Inspection Institute, Hohhot 010070 (China); Xin, Xiao-Dong; Guo, Feng; Cao, Xiao-Fang [College of Chemistry and Chemical Engineering, Inner Mongolia University, Hohhot 010021 (China)

2015-06-15

Two novel solid binary complexes of rare earth perchlorate with phenacyl p-tolyl sulfoxide were synthesized and characterized by elemental analysis, molar conductivity, coordination titration analysis, IR, TG-DSC, {sup 1}HNMR and UV spectra. The results indicated that the composition of these complexes was REL{sub 7} (ClO{sub 4}){sub 3}·6H{sub 2}O (RE=Eu (III), Tb (III), L=C{sub 6}H{sub 5}COCH{sub 2}SOC{sub 6}H{sub 4}CH{sub 3}). The study on IR spectra and {sup 1}HNMR spectra revealed that phenacyl p-tolyl sulfoxide bonded with RE{sup 3+} ions by the oxygen atom in sulfinyl group. The emission spectra illustrated that both the Eu (III) and Tb (III) complexes displayed excellent luminescence in solid state, and The most intensive characteristic emission of the Eu(III) and Tb(III) complexes were 245,400 a.u. and 298,000 a.u. respectively. The slit with was 1 nm. By analysis luminescence and phosphorescence spectrum, it was found that the ligand had the advantage to absorb energy and transfer it to the Eu (III) and Tb (III) ions. The fluorescence lifetimes of the complexes were measured as well as the quantum yield of the Eu (III) complex.

Molecular dynamics simulations of ter-pyridine and bis-triazinyl-pyridine complexes with lanthanide cations; Etude de dynamique moleculaire de complexes de la bis-triazinyl-pyridine (BTP) et de la terpyridine avec des lanthanides(3)

Energy Technology Data Exchange (ETDEWEB)

Guilbaud, Ph. [CEA Valrho, (DCC/DRRV/SEMP), 30 - Marcoule (France)

2000-07-01

The search for ligands which specifically separate actinides(III) from lanthanides(III) by liquid-liquid extraction has prompted considerable research in the Process Design and Modeling Department ('Service d'Etude et de Modelisation des Procedes'- SEMP). Ligands with soft donor atoms AS) that are able to perform this separation have already been investigated and research is currently under way to improve their performance for high acidic feeds. Theoretical chemistry research is conducted in the Theoretical and Structural Chemistry Laboratory ('Laboratoire de Chimie Theorique et Structurale') to improve our understanding of the complexation and extraction of these cations with such ligands. Theoretical studies were first carried out for the ter-pyridine (TPY) and bis-triazinyl-pyridine (BTP) ligands that display fairly good ability to separate and extract actinide(III) from lanthanide(III) ions. Molecular dynamics simulations were performed on ter-pyridine and bis-triazinyl-pyridine complexes with three lanthanide cations (La{sup 3+}, Eu{sup 3+} and Lu{sup 3+}) for vacuum and for water solutions. These calculations were carried out without counter-ions, with three nitrate (NO{sub 3}{sup -}) ions, and, in the case of ter-pyridine, with three {alpha}-bromo-caprate anions that are likely to be used experimentally as synergistic agents for the separation and extraction of An(III) from Ln(III). Molecular dynamics simulations were first performed for vacuum to evaluate the distances between nitrogen and lanthanide atoms (Ln{sup 3+},N) and intrinsic interaction energies to poly-nitrogenous ligands with or without NO{sub 3} ions, and for both ligands. The (Ln{sup 3+},N) distances decrease and the cation/ligand interaction energies increase along the La{sup 3+}, Eu{sup 3+}, Lu{sup 3+} series, with decreasing Ln(III) ion radii. The introduction of nitrate counter-ions makes the (Ln{sup 3+},N) distances slightly higher, and the TPY/Ln{sup 3+} and BTP

Cloud point extraction: an alternative to traditional liquid-liquid extraction for lanthanides(III) separation.

Science.gov (United States)

Favre-Réguillon, Alain; Draye, Micheline; Lebuzit, Gérard; Thomas, Sylvie; Foos, Jacques; Cote, Gérard; Guy, Alain

2004-06-17

Cloud point extraction (CPE) was used to extract and separate lanthanum(III) and gadolinium(III) nitrate from an aqueous solution. The methodology used is based on the formation of lanthanide(III)-8-hydroxyquinoline (8-HQ) complexes soluble in a micellar phase of non-ionic surfactant. The lanthanide(III) complexes are then extracted into the surfactant-rich phase at a temperature above the cloud point temperature (CPT). The structure of the non-ionic surfactant, and the chelating agent-metal molar ratio are identified as factors determining the extraction efficiency and selectivity. In an aqueous solution containing equimolar concentrations of La(III) and Gd(III), extraction efficiency for Gd(III) can reach 96% with a Gd(III)/La(III) selectivity higher than 30 using Triton X-114. Under those conditions, a Gd(III) decontamination factor of 50 is obtained.

Thermodynamic approach of the poly-azine - f element ions interaction in aqueous conditions

International Nuclear Information System (INIS)

Miguirditchian, M.; Guillaumont, D.; Moisy, P.; Guillaneux, D.; Madic, C.

2004-01-01

2-Amino-4,6-di-(pyridine-2-yl)-1,3,5-triazine (Adptz) was considered as a model compound for selective aromatic nitrogen extractants (poly-azines) of minor actinides. Thermodynamic data ( ΔG 0 , ΔH 0 , ΔS 0 ) were systematically acquired for the complexation of lanthanide(III) ions as well as yttrium(III) and americium(III) in hydro-alcoholic medium. Two complementary experimental approaches were followed. Stability constants for the formation of the 1:1 complexes were evaluated from UV-visible spectrophotometry titration experiments, whereas enthalpies and entropies of reaction were obtained consistently from either temperature dependence experiments or micro-calorimetry. The interaction of Adptz with lanthanide(III) and yttrium(III) ions was found to be essentially ionic and dependent upon the hydration and size of the ion. As for americium(III) ion, stability constant and enthalpy of complexation was significantly larger. This was attributed to a partial electronic transfer from the ligand to empty orbitals of the cation. DFT calculations support this interpretation. (authors)

Synthesis, characterization and magnetic properties of novel μ-oxamido heterodinuclear copper(II) - lanthanide(III) complexes

International Nuclear Information System (INIS)

Li, Y.T.; Miao, M.M.; Liao, D.Z.; Jiang, Z.H.; Wang, G.L.

1995-01-01

Six novel μ-oxamido heterobinuclear complexes have been prepared and identified as Cu(oxpn)Ln(L) 2 (ClO 4 ) 3 , where oxpn denotes the N, N'-bis(3-aminopropyl)oxamido dianion, L, 1,10-phenanthroline (phen) and Ln stands for La, Nd, Gd, Tb, Ho, Er. The complexes Cu(oxpn)Gd(oxpn)Gd(phen) 2 (ClO 4 ) 3 were characterized with variable temperature magnetic susceptibility (4-300 K). The exchange integral J (Cu-Gd) was found to be 2.03 cm -1 . The result is commensurate with ferromagnetic interaction between the adjacent metal ions. One plausible mechanism that can cause a ferromagnetic coupling between Gd(III) and Cu(II) is also discussed in terms of spin polarized. (author). 32 refs, 3 figs, 3 tabs

Mechanochemically assisted solid-state and citric acid complex syntheses of Cu-doped sodium cobaltite ceramics

International Nuclear Information System (INIS)

Pršić, S.; Savić, S.M.; Branković, Z.; Vrtnik, S.; Dapčević, A.; Branković, G.

2015-01-01

Highlights: • Sodium cobaltite was synthesized by mechanochemically assisted solid-state reaction and citric acid complex (CAC) method. • We investigated effect of Cu-doping in NaCo 2−x Cu x O 4 (x = 0, 0.01, 0.03, 0.05). • ICP analysis showed that the controlling of the samples composition is easier by the CAC method. • The Seebeck coefficient in Cu-doped samples was higher compared to the undoped one. • The highest figure of merit was observed in the sample with the lowest Cu concentration. - Abstract: In the last decade, the sodium cobaltite ceramic became a promising candidate for potential thermoelectric applications, because of its large thermopower and low resistivity. In this work, polycrystalline samples of NaCo 2−x Cu x O 4 (x = 0, 0.01, 0.03, 0.05) were prepared using mechanochemically assisted solid-state reaction method (MASSR) and the citric acid complex method (CAC). Bulk samples were prepared by pressing into disc-shaped pellets and subsequently subjected to a thermal treatment at 880 °C in inert argon atmosphere. Changes in structural and microstructural characteristics of the samples, caused by the substitution of Cu for Co, were characterized using X-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM), respectively. The results of inductively coupled plasma (ICP) analysis showed that the compositions of the final products correspond to γ-NaCo 2 O 4 and confirmed that desired compound was obtained in both syntheses procedures. The advantages and disadvantages of these two syntheses procedures have been observed and discussed: the CAC method enabled obtaining samples with higher density and fine microstructure compared to the MASSR method, thus better thermoelectric properties. The Cu 2+ substitution led to the increase in Seebeck coefficient in both synthesis routes. The highest figure of merit of 0.022 at 300 K was observed for the sample doped with 1 mol% Cu, obtained by the CAC method, and it was almost twice

Mechanochemically assisted solid-state and citric acid complex syntheses of Cu-doped sodium cobaltite ceramics

Energy Technology Data Exchange (ETDEWEB)

Pršić, S., E-mail: sanjaprsic@imsi.bg.ac.rs [Institute for Multidisciplinary Research, University of Belgrade, Kneza Višeslava 1, 11030 Belgrade (Serbia); Savić, S.M., E-mail: slavicas@imsi.bg.ac.rs [Institute for Multidisciplinary Research, University of Belgrade, Kneza Višeslava 1, 11030 Belgrade (Serbia); Branković, Z., E-mail: zorica.brankovic@imsi.bg.ac.rs [Institute for Multidisciplinary Research, University of Belgrade, Kneza Višeslava 1, 11030 Belgrade (Serbia); Vrtnik, S., E-mail: stane.vrtnik@ijs.si [Institute Jožef Stefan, Condensed Matter Physics, Jamova cesta 39, 1000 Ljubljana (Slovenia); Dapčević, A., E-mail: hadzi-tonic@tmf.bg.ac.rs [Department of General and Inorganic Chemistry, Faculty of Technology and Metallurgy, University of Belgrade, Karnegijeva 4, 11120 Belgrade (Serbia); Branković, G., E-mail: goran.brankovic@imsi.bg.ac.rs [Institute for Multidisciplinary Research, University of Belgrade, Kneza Višeslava 1, 11030 Belgrade (Serbia)

2015-08-15

Highlights: • Sodium cobaltite was synthesized by mechanochemically assisted solid-state reaction and citric acid complex (CAC) method. • We investigated effect of Cu-doping in NaCo{sub 2−x}Cu{sub x}O{sub 4} (x = 0, 0.01, 0.03, 0.05). • ICP analysis showed that the controlling of the samples composition is easier by the CAC method. • The Seebeck coefficient in Cu-doped samples was higher compared to the undoped one. • The highest figure of merit was observed in the sample with the lowest Cu concentration. - Abstract: In the last decade, the sodium cobaltite ceramic became a promising candidate for potential thermoelectric applications, because of its large thermopower and low resistivity. In this work, polycrystalline samples of NaCo{sub 2−x}Cu{sub x}O{sub 4} (x = 0, 0.01, 0.03, 0.05) were prepared using mechanochemically assisted solid-state reaction method (MASSR) and the citric acid complex method (CAC). Bulk samples were prepared by pressing into disc-shaped pellets and subsequently subjected to a thermal treatment at 880 °C in inert argon atmosphere. Changes in structural and microstructural characteristics of the samples, caused by the substitution of Cu for Co, were characterized using X-ray diffraction (XRD) analysis, and scanning electron microscopy (SEM), respectively. The results of inductively coupled plasma (ICP) analysis showed that the compositions of the final products correspond to γ-NaCo{sub 2}O{sub 4} and confirmed that desired compound was obtained in both syntheses procedures. The advantages and disadvantages of these two syntheses procedures have been observed and discussed: the CAC method enabled obtaining samples with higher density and fine microstructure compared to the MASSR method, thus better thermoelectric properties. The Cu{sup 2+} substitution led to the increase in Seebeck coefficient in both synthesis routes. The highest figure of merit of 0.022 at 300 K was observed for the sample doped with 1 mol% Cu, obtained by

Molecular nanomagnets: Syntheses and characterization of high nuclearity transition metal complexes

Science.gov (United States)

Foguet-Albiol, Maria D.

2006-12-01

High nuclearity transition metal complexes have attracted a lot of attention because of their aesthetically pleasant structures and/or their potential applications. The fusion of the world of magnetism with the exciting research in physics and chemistry led to the realization of interesting types of materials that can function as nanoscale magnetic particles. The study of the magnetism of inorganic complexes and especially the study of these molecular nanomagnets (or single-molecule magnets, SMMs) is a field that has generated intense interest in the scientific community. Interest in these molecular nanomagnets arises as part of a broader investigation of nanomagnetism (and nanotechnology), as these represent the ultimate step in device miniaturization. The primary purpose of this dissertation is the development of new synthetic methods intended for the preparation of novel single-molecule magnets (SMMs). The definition of the "bottom-up approach" is to increase the size of molecules by adding new magnetic centers; this is attractive but does not actually reflect how the chemistry takes place. Various strategies have been employed in developing the aforementioned synthetic methods which include the use of mononuclear as well as preformed clusters as starting materials; and the introduction of new alcohol based ligands as N-methyldiethanolamine (mdaH2) and triethanolamine (teaH3), since currently only a few alcohol based ligands have been used by different research groups. Many of these efforts have led to the isolation of new polynuclear Mn clusters with nuclearities ranging all the way from four to thirty-one. Additionally, a family of related Fe7 complexes has been synthesized. The transition metal cluster chemistry has also been extended to nickel-containing species. Many of these polynulear transition metal complexes function as single-molecule magnets. An additional research direction discussed herein is the study of the exchange-coupled dimer of single

Inner-sphere and outer-sphere complexes of yttrium(III), lanthanum (III), neodymium(III), terbium(III) and thulium(III) with halide ions in N,N-dimethylformamide

International Nuclear Information System (INIS)

Takahashi, Ryouta; Ishiguro, Shin-ichi

1991-01-01

The formation of chloro, bromo and iodo complexes of yttrium(III), and bromo and iodo complexes of lanthanum(III), neodymium(III), terbium(III) and thulium(III) has been studied by precise titration calorimetry in N,N-dimethylformamide (DMF) at 25 o C. The formation of [YCl] 2+ , [YCl 2 ] + , [YCl 3 ] and [YCl 4 ] - , and [MBr] 2+ and [MBr 2 ] + (M = Y, La, Nd, Tb, Tm) was revealed, and their formation constants, enthalpies and entropies were determined. It is found that the formation enthalpies change in the sequence ΔH o (Cl) > ΔH o (l), which is unusual for hard metal (III) ions. This implies that, unlike the chloride ion, the bromide ion forms outer-sphere complexes with the lanthanide(III) and yttrium(III) ions in DMF. Evidence for either an inner- or outer-sphere complex was obtained from 89 Y NMR spectra for Y(ClO 4 ) 3 , YCl 3 and YBr 3 DMF solutions at room temperature. (author)

Novel heterometallic metal–azido complex synthesized by “one-step” reaction: synthetic strategy and magnetic properties

Energy Technology Data Exchange (ETDEWEB)

Jiao, Yong-Kun [School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Xiu-Ping [Technical center for safety of industrial products of Tianjin entry-exit inspection and quarantine bureau, Tianjin 300201 (China); Zhao, Cui; Wang, Hai-Chao; Xue, Min [School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Zhao, Jiong-Peng, E-mail: horryzhao@yahoo.com [School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Liu, Fu-Chen, E-mail: fuchenliutj@yahoo.com [School of Chemistry and Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Lanzhou Petrochemical College of Vocational Technology, Lanzhou 730060 (China)

2013-06-15

A novel heterometallic complex, [Ni{sub 2}Mn(N{sub 3}){sub 2}(nic){sub 4}·(H{sub 2}O){sub 2}]{sub n} (1) (nic=nicotinate), was obtained by assembling MnCl{sub 2}·4H{sub 2}O, Ni(NO{sub 3}){sub 2}·6H{sub 2}O, NaN{sub 3} and nicotinic acid with a “one step” synthetic strategy—hydrothermal reaction. The 3D structure of the complex can be described as end-on (EO) azido and syn,syn carboxylates mixed bridged by alternate Ni–Mn–Ni trimers linked by the nicotinate. Dominant ferromagnetic interactions were observed between the Ni{sup II} and Mn{sup II} ions in the trimer. - Graphical abstract: A novel heterometallic 3D complex [Ni{sub 2}Mn(N{sub 3}){sub 2}(nic){sub 4}·(H{sub 2}O){sub 2}]{sub n} (1) (nic=nicotinate) was synthesized by hydrothermal reaction. This complex exhibits interesting structural and magnetic properties. - Highlights: • It is difficult to construct simple coordination complexes with azide as “ligands” to obtain heterometallic metal–azido compounds. • A “one-step” method—hydrothermal reaction— was introduced to avoid the disadvantages of azide mentioned above. • The magnetic property is different with the isostructural homometal–azido complex due to the changed metal center.

Magnetic properties of cyano-bridged Ln3+-M3+ complexes. Part I: trinuclear complexes (Ln3+ = La, Ce, Pr, Nd, Sm; M3+ = FeLS, Co) with bpy as blocking ligand.

Science.gov (United States)

Figuerola, Albert; Ribas, Joan; Llunell, Miquel; Casanova, David; Maestro, Miguel; Alvarez, Santiago; Diaz, Carmen

2005-10-03

The reaction of Ln(NO3)3(aq) with K3[Fe(CN)6] or K3[Co(CN)6] and 2,2'-bipyridine in water/ethanol led to eight trinuclear complexes: trans-[M(CN)4(mu-CN)2{Ln(H2O)4(bpy)2}2][M(CN)6].8H2O (M = Fe3+ or Co3+, Ln = La3+, Ce3+, Pr3+, Nd3+, and Sm3+). The structures for the eight complexes [La2Fe] (1), [Ce2Fe] (2), [Pr2Fe] (3), [Nd2Fe] (4), [Ce2Co] (5), [Pr2Co] (6), [Nd2Co] (7), and [Sm2Co] (8) have been solved; they crystallize in the triclinic space group P and are isomorphous. They exhibit a supramolecular 3D architecture through hydrogen bonding and pi-pi stacking interactions. A stereochemical study of the nine-vertex polyhedra of the lanthanide ions, based on continuous shape measures, is presented. No significant magnetic interaction was found between the lanthanide(III) and the iron(III) ions.

Syntheses, structural elucidation, thermal properties, theoretical quantum chemical studies (DFT and biological studies of barbituric–hydrazone complexes

Directory of Open Access Journals (Sweden)

Amina A. Soayed

2015-03-01

Full Text Available Condensation of barbituric acid with hydrazine hydrate yielded barbiturichydrazone (L which was characterized using IR, 1H NMR and mass spectra. The Co(II, Ni(II and Cu(II complexes derived from this ligand have been synthesized and structurally characterized by elemental analyses, spectroscopic methods (IR, UV–Vis and ESR and thermal analyses (TGA, DTG and DTA and the structures were further elucidated using quantum chemical density functional theory. Complexes of L were found to have the ML.nH2O stoichiometry with either tetrahedral or octahedral geometry. The ESR data showed the Cu(II complex to be in a tetragonal geometry. Theoretical investigation of the electronic structure of metal complexes at the TD-DFT/B3LYP level of theory has been carried out and discussed. The fundamental vibrational wavenumbers were calculated and a good agreement between observed and scaled calculated wavenumbers was achieved. Thermal studies were performed to deduce the stabilities of the ligand and complexes. Thermodynamic parameters, such as the order of reactions (n, activation energy ΔE∗, enthalpy of reaction ΔH∗ and entropy ΔS∗ were calculated from DTA curves using Horowitz–Metzger method. The ligand L and its complexes have been screened for their antifungal and antibacterial activities and were found to possess better biological activities compared to those of unsubstituted barbituric acid complexes.

Quantum mechanics and molecular dynamics simulations of complexation of alkaline-earth and lanthanide cations by poly-amino-carboxylate ligands

International Nuclear Information System (INIS)

Durand, S.

1999-01-01

Molecular dynamics (MD) simulations on lanthanide(III) and alkaline-earth(II) complexes with poly-amino-carboxylates (ethylene-diamino-tetra-acetate EDTA 4- , ethylene-diamino-tri-acetate-acetic acid EDTA(H) 3- , tetra-aza-cyclo-dodecane-tetra-acetate DOTA 4- , methylene-imidine-acetate MIDA 2- ) are reported. First, a consistent set of Lennard-Jones parameters for La 3+ , Eu 3+ and Lu 3+ cations has been derived from free energy calculations in aqueous solution. Observed differences in hydration free energies, coordination distances and hydration numbers are reproduced. Then, the solution structures of 1:1 complexes of alkaline-earth and/or lanthanide cations with EDTA 4- , EDTA(H) 3- , DOTA 4- and 1:2 complexes of lanthanide cations with MIDA 2- were studied by MD in water. In addition, free energy calculations were performed to study, for each ligand, the relative thermodynamic stabilities of complexes with Ca 2+ vs Sr 2+ and vs Ba 2+ on the one hand, and with La 3+ vs Eu 3+ and vs Lu 3+ on the other hand. Model does not take into account explicitly polarization and charge transfer. However, the results qualitatively agree with experimental complexation data (structure and selectivities). (author)

hydrazines and their nickel(II) complexes: Syntheses, structures and ...

Indian Academy of Sciences (India)

G Narendra Babu

Abstract. The Schiff bases N-(acyl)-N -(ferrocenylidene)hydrazines (HFcah (1) and HFcbh (2), where acyl = acetyl in 1 and benzoyl in 2 and H represents the dissociable amide proton) were synthesized in high yields (74 and 81%) by condensation reactions of equimolar amounts of ferrocene-carboxaldehyde and the ...

Lanthanide(III) complexes with tridentate Schiff base ligand ...

African Journals Online (AJOL)

The X-ray study reveals isotopic Nd/Sm binuclear structures were each metal ion is nine-coordinated in the same fashion. Both metal centers have distorted tricapped trigonal prism geometry, with the Schiff base acting as tridentate ligand. The DPPH· radical scavenging effects of the Schiff base ligand and its Ln(III) ...

Electrocatalytic Activity and Stability of M-Fe Catalysts Synthesized by Polymer Complex Method for PEFC Cathode

KAUST Repository

Ou, Yiwei

2011-11-01

The polymerized complex (PC) method was used to synthesize highly dispersed iron-based catalysts for the oxygen reduction reaction (ORR). The catalysts were prepared with an addition of 1,10-phenanthroline (Phen) and transition metals (M), such as Ta, Ti, and W, in an attempt to enhance the ORR activity and durability of the catalysts. The composition and properties of the catalysts were characterized by thermogravimetric analysis, X-ray diffraction, and X-ray photoelectron spectroscopy. The catalyst components, after extensive dissolution in a strong acid solution, were characterized by inductively coupled plasma mass spectroscopy and ultraviolet-visible spectroscopy. It was found that the Ti-Fe catalyst showed improved ORR performance, and the Ta-Fe catalyst showed enhanced stability towards ORR in acidic solution. The catalytic activity and stability for ORR was observed by adding Ti or Ta into the catalyst formulation, suggesting that the interaction between added hetero-ions (Ti and Ta) and ionic Fe active sites was beneficial for the ORR. A single-cell test with the synthesized catalyst in the cathode initially generated a high power density, but the low stability remains an issue to be solved.

Electrocatalytic Activity and Stability of M-Fe Catalysts Synthesized by Polymer Complex Method for PEFC Cathode

KAUST Repository

Ou, Yiwei; Kumagai, Hiromu; Yin, Fengxiang; Okada, Saori; Hatasawa, Haruna; Morioka, Hiroyuki; Takanabe, Kazuhiro; Kubota, Jun; Domen, Kazunari

2011-01-01

The polymerized complex (PC) method was used to synthesize highly dispersed iron-based catalysts for the oxygen reduction reaction (ORR). The catalysts were prepared with an addition of 1,10-phenanthroline (Phen) and transition metals (M), such as Ta, Ti, and W, in an attempt to enhance the ORR activity and durability of the catalysts. The composition and properties of the catalysts were characterized by thermogravimetric analysis, X-ray diffraction, and X-ray photoelectron spectroscopy. The catalyst components, after extensive dissolution in a strong acid solution, were characterized by inductively coupled plasma mass spectroscopy and ultraviolet-visible spectroscopy. It was found that the Ti-Fe catalyst showed improved ORR performance, and the Ta-Fe catalyst showed enhanced stability towards ORR in acidic solution. The catalytic activity and stability for ORR was observed by adding Ti or Ta into the catalyst formulation, suggesting that the interaction between added hetero-ions (Ti and Ta) and ionic Fe active sites was beneficial for the ORR. A single-cell test with the synthesized catalyst in the cathode initially generated a high power density, but the low stability remains an issue to be solved.

Influence of calcination temperature on the zirconia microstructure synthesized by complex polymerization method (CPM): a comparative study

Energy Technology Data Exchange (ETDEWEB)

Santos, R.L.P.; Mota, F.V.; Nascimento, R.M.; Henriques, B.P.; Silva, F.S.; Assis, R. [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil)

2016-07-01

Full text: The aim of this study was to accomplish a previous characterization of the zirconia synthesized by Complex Polymerization Method (CPM) using yttria as stabilizing agent and different calcination temperatures. The powders were crystallized at 800, 900 and 1000 °C for 2h. The structural evolution Y-TZP powders were characterized by X-Ray Diffraction (XRD) and Micro-Raman Spectroscopy. The thermal properties of the calcined pre-pyrolyzed (350 °C for 4 h), samples were investigated by simultaneous thermo analysis (TGA/DTA). After heat treatment the phase Y-TZP was obtained of a single-phase, with absence of the deleterious phases. The results show that average crystallite size of the powder synthesized with 3% of Yttria dopant, increased from 11.5 to 27.9 nm when the calcination temperature increased from 800 to 1000 °C. This behavior was observed for all specimens independent of the Yttria content. The micro-Raman indicate the presence of the tetragonal phase for all samples independent of the calcination temperature employed. (author)

Syntheses, molecular and crystalline architectures, and ...

Indian Academy of Sciences (India)

Syntheses, molecular and crystalline architectures, and luminescence behaviour of terephthalate bridged heptacoordinated dinuclear lead(II) complexes containing a pentadentate N-donor Schiff base. SUBHASIS ROYa, SOMNATH CHOUBEYa, SUMITAVA KHANa, KISHALAY BHARa,. PARTHA MITRAb and BARINDRA ...

Quantum mechanics and molecular dynamics simulations of complexation of alkaline-earth and lanthanide cations by poly-amino-carboxylate ligands; Simulations par mecanique quantique et dynamique moleculaire de la complexation de cations alcalino-terreux et lanthanides par des ligands polyaminocarboxylates

Energy Technology Data Exchange (ETDEWEB)

Durand, S

1999-07-01

Molecular dynamics (MD) simulations on lanthanide(III) and alkaline-earth(II) complexes with poly-amino-carboxylates (ethylene-diamino-tetra-acetate EDTA{sup 4-}, ethylene-diamino-tri-acetate-acetic acid EDTA(H){sup 3-}, tetra-aza-cyclo-dodecane-tetra-acetate DOTA{sup 4-}, methylene-imidine-acetate MIDA{sup 2-}) are reported. First, a consistent set of Lennard-Jones parameters for La{sup 3+}, Eu{sup 3+} and Lu{sup 3+} cations has been derived from free energy calculations in aqueous solution. Observed differences in hydration free energies, coordination distances and hydration numbers are reproduced. Then, the solution structures of 1:1 complexes of alkaline-earth and/or lanthanide cations with EDTA{sup 4-}, EDTA(H){sup 3-}, DOTA{sup 4-} and 1:2 complexes of lanthanide cations with MIDA{sup 2-} were studied by MD in water. In addition, free energy calculations were performed to study, for each ligand, the relative thermodynamic stabilities of complexes with Ca{sup 2+} vs Sr{sup 2+} and vs Ba{sup 2+} on the one hand, and with La{sup 3+} vs Eu{sup 3+} and vs Lu{sup 3+} on the other hand. Model does not take into account explicitly polarization and charge transfer. However, the results qualitatively agree with experimental complexation data (structure and selectivities). (author)

Syntheses, crystal structures and spectroscopic properties of copper(II)-tetracyanometallate(II) complexes with nicotinamide and isonicotinamide ligands

Science.gov (United States)

Sayın, Elvan; Kürkçüoğlu, Güneş Süheyla; Yeşilel, Okan Zafer; Hökelek, Tuncer

2015-09-01

Four new one dimensional (1D) cyanide complexes, namely {[Cu(NH3)4(μ-na)][M‧(CN)4]}n and {[Cu(NH3)2(ina)2M‧(μ-CN)2(CN)2]}n (M‧(II) = Pd (1 and 3) or Pt (2 and 4), na:nicotinamide and ina:isonicotinamide) have been synthesized and characterized by elemental, spectral (FT-IR and Raman), and thermal (TG, DTG and DTA) analyses. The crystal structures of complexes 1-3 have been determined by single crystal X-ray diffraction technique. In complexes 1 and 2, na ligand is coordinated to the adjacent Cu(II) ions as a bridging ligand, giving rise to 1D linear cationic chain and the [M‧(CN)4]2- anionic complex acts as a counter ion. Complexes 3 and 4 are also 1D linear chain in which two cyanide ligands bridged neighboring M‧(II) and Cu(II) ions, while ina ligand is coordinated Cu(II) ion through nitrogen atom of pyridine ring. In the complexes, the Cu(II) ions adopt distorted octahedral geometries, while M‧(II) ions are four coordinated with four carbon atoms from cyanide ligands in square-planar geometries. The adjacent chains are further stacked through intermolecular hydrogen bond, Nsbnd Hṡṡṡπ, Csbnd H⋯M‧ and M‧⋯π interactions to form 3D supramolecular networks. Vibration assignments are given for all the observed bands. In addition, thermal stabilities of the compounds are also discussed.

A series of 2D metal-quinolone complexes: Syntheses, structures, and physical properties

Energy Technology Data Exchange (ETDEWEB)

He, Jiang-Hong [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Xiao, Dong-Rong, E-mail: xiaodr98@yahoo.com.cn [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Chen, Hai-Yan; Sun, Dian-Zhen; Yan, Shi-Wei; Wang, Xin; Ye, Zhong-Li [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Luo, Qun-Li, E-mail: qlluo@swu.edu.cn [College of Chemistry and Chemical Engineering, Southwest University, Chongqing 400715 (China); Wang, En-Bo, E-mail: wangeb889@nenu.edu.cn [Key Laboratory of Polyoxometalate Science of Ministry of Education, Department of Chemistry, Northeast Normal University, Changchun 130024 (China)

2013-02-15

Six novel 2D metal-quinolone complexes, namely [Cd(cfH)(bpdc)]{center_dot}H{sub 2}O (1), [M(norfH)(bpdc)]{center_dot}H{sub 2}O (M=Cd (2) and Mn (3)), [Mn{sub 2}(cfH)(odpa)(H{sub 2}O){sub 3}]{center_dot}0.5H{sub 2}O (4), [Co{sub 2}(norfH)(bpta)({mu}{sub 2}-H{sub 2}O)(H{sub 2}O){sub 2}]{center_dot}H{sub 2}O (5) and [Co{sub 3}(saraH){sub 2}(Hbpta){sub 2}(H{sub 2}O){sub 4}]{center_dot}9H{sub 2}O (6) (cfH=ciprofloxacin, norfH=norfloxacin, saraH=sarafloxacin, bpdc=4,4 Prime -biphenyldicarboxylate, odpa=4,4 Prime -oxydiphthalate, bpta=3,3 Prime ,4,4 Prime -biphenyltetracarboxylate) have been synthesized and characterized. Compounds 1-3 consist of 2D arm-shaped layers based on the 1D {l_brace}M(COO){r_brace}{sub n}{sup n+} chains. Compounds 4 and 5 display 2D structures based on tetranuclear manganese or cobalt clusters with (3,6)-connected kgd topology. Compound 6 exhibits a 2D bilayer structure, which represents the first example of metal-quinolone complexes with 2D bilayer structure. By inspection of the structures of 1-6, it is believed that the long aromatic polycarboxylate ligands are important for the formation of 2D metal-quinolone complexes. The magnetic properties of compounds 3-6 was studied, indicating the existence of antiferromagnetic interactions. Furthermore, the luminescent properties of compounds 1-2 are discussed. - Graphical abstract: Six novel 2D metal-quinolone complexes have been prepared by self-assemblies of the quinolones and metal salts in the presence of long aromatic polycarboxylates. Highlights: Black-Right-Pointing-Pointer Compounds 1-3 consist of novel 2D arm-shaped layers based on the 1D {l_brace}M(COO){r_brace}{sub n}{sup n+} chains. Black-Right-Pointing-Pointer Compounds 4 and 5 are two novel 2D layers based on tetranuclear Mn or Co clusters with kgd topology. Black-Right-Pointing-Pointer Compound 6 is the first example of metal-quinolone complexes with 2D bilayer structure. Black-Right-Pointing-Pointer Compounds 1-6 represent six unusual

Aeon: Synthesizing Scheduling Algorithms from High-Level Models

Science.gov (United States)

Monette, Jean-Noël; Deville, Yves; van Hentenryck, Pascal

This paper describes the aeon system whose aim is to synthesize scheduling algorithms from high-level models. A eon, which is entirely written in comet, receives as input a high-level model for a scheduling application which is then analyzed to generate a dedicated scheduling algorithm exploiting the structure of the model. A eon provides a variety of synthesizers for generating complete or heuristic algorithms. Moreover, synthesizers are compositional, making it possible to generate complex hybrid algorithms naturally. Preliminary experimental results indicate that this approach may be competitive with state-of-the-art search algorithms.

Singlet Energy Transfer as the Main Pathway in the Sensitization of Near-Infrared Nd3+ Luminescence by Dansyl and Lissamine Dyes

NARCIS (Netherlands)

Hebbink, G.A.; Klink, S.I.; Grave, Lennart; Oude Alink, Patrick G.B.; van Veggel, F.C.J.M.

2002-01-01

general, sensitization of lanthanide(III) ions by organic sensitizers is regarded to take place via the triplet state of the sensitizers. Herein, we show that in dansyl- and lissamine-functionalized Nd3+ complexes energy transfer occurs from the singlet state of the sensitizers to the Nd3+ center.

Investigation of formation constant of complex of a new synthesized tripodal ligand with Cu2+ using rank annihilation factor analysis in surfactant media

Directory of Open Access Journals (Sweden)

R. Golbedaghi

2014-01-01

Full Text Available The complex formation between a newly synthesized tripodal ligand and the cation Cu2+ in water and surfactant media was studied spectrophotometrically using rank annihilation factor analysis (RAFA. According to molar ratio data the stoichiometry of complexation between the ligand and the cation Cu2+ was 1:1. Formation constant of this complex was derived using RAFA on spectrophotometric data. The performance of the method has been evaluated by using synthetic data. Also concentration and spectral profiles of ligand and complex can be obtained by using the stability constant and appropriate equations. The effect of surfactants such as sodium dodecyl sulfate (SDS, cetyltrimethylammonium bromide (CTAB and Triton X-100 on complex formation constant of Cu2+ with the ligand was investigated.

The Human Nuclear Exosome Targeting Complex Is Loaded onto Newly Synthesized RNA to Direct Early Ribonucleolysis

Directory of Open Access Journals (Sweden)

Michal Lubas

2015-01-01

Full Text Available The RNA exosome complex constitutes the major nuclear eukaryotic 3′-5′ exonuclease. Outside of nucleoli, the human nucleoplasmic exosome is directed to some of its substrates by the nuclear exosome targeting (NEXT complex. How NEXT targets RNA has remained elusive. Using an in vivo crosslinking approach, we report global RNA binding sites of RBM7, a key component of NEXT. RBM7 associates broadly with RNA polymerase II-derived RNA, including pre-mRNA and short-lived exosome substrates such as promoter upstream transcripts (PROMPTs, enhancer RNAs (eRNAs, and 3′-extended products from snRNA and replication-dependent histone genes. Within pre-mRNA, RBM7 accumulates at the 3′ ends of introns, and pulse-labeling experiments demonstrate that RBM7/NEXT defines an early exosome-targeting pathway for 3′-extended snoRNAs derived from such introns. We propose that RBM7 is generally loaded onto newly synthesized RNA to accommodate exosome action in case of available unprotected RNA 3′ ends.

Evaluation of DNA, BSA binding, and antimicrobial activity of new synthesized neodymium complex containing 29-dimethyl 110-phenanthroline.

Science.gov (United States)

Moradi, Zohreh; Khorasani-Motlagh, Mozhgan; Rezvani, Ali Reza; Noroozifar, Meissam

2018-02-01

In order to evaluate biological potential of a novel synthesized complex [Nd(dmp) 2 Cl 3 .OH 2 ] where dmp is 29-dimethyl 110-phenanthroline, the DNA-binding, cleavage, BSA binding, and antimicrobial activity properties of the complex are investigated by multispectroscopic techniques study in physiological buffer (pH 7.2).The intrinsic binding constant (K b ) for interaction of Nd(III) complex and FS-DNA is calculated by UV-Vis (K b  = 2.7 ± 0.07 × 10 5 ) and fluorescence spectroscopy (K b  = 1.13 ± 0.03 × 10 5 ). The Stern-Volmer constant (K SV ), thermodynamic parameters including free energy change (ΔG°), enthalpy change (∆H°), and entropy change (∆S°), are calculated by fluorescent data and Vant' Hoff equation. The experimental results show that the complex can bind to FS-DNA and the major binding mode is groove binding. Meanwhile, the interaction of Nd(III) complex with protein, bovine serum albumin (BSA), has also been studied by using absorption and emission spectroscopic tools. The experimental results show that the complex exhibits good binding propensity to BSA. The positive ΔH° and ∆S° values indicate that the hydrophobic interaction is main force in the binding of the Nd(III) complex to BSA, and the complex can quench the intrinsic fluorescence of BSA remarkably through a static quenching process. Also, DNA cleavage was investigated by agarose gel electrophoresis that according to the results cleavage of DNA increased with increasing of concentration of the complex. Antimicrobial screening test gives good results in the presence of Nd(III) complex system.

Determination of the formation constant for the inclusion complex between Lanthanide ions and Dansyl chloride derivative by fluorescence spectroscopy: Theoretical and experimental investigation

Science.gov (United States)

Riahi, Siavash; Ganjali, Mohammad Reza; Hariri, Maryam; Abdolahzadeh, Shaghayegh; Norouzi, Parviz

2009-09-01

In this paper, a sensitive, easy, efficient, and suitable method for the calculation of Kf values of complexation between one derivative of Dansyl chloride [5-(dimethylamino) naphthalene-1-sulfonyl 4-phenylsemicarbazide] (DMNP) and Lanthanide(III) (Ln) ions is proposed, using both spectrofluorometric and spectrophotometric methods. Determination of Kf showed that DMNP was mostly selective towards the erbium (III) ion. The validity of the method was also confirmed calculating the Stern-Volmer fluorescence quenching constants ( Ksv) that resulted in the same consequence, obtained by calculating the Kf of complexation values. In addition, the UV-vis spectroscopy was applied for the determination of Kf only for the Ln ions that had interactions with DMNP. Finally, the DFT studies were done on Er 3+ and the DMNP complex for distinguishing the active sites and estimating the pair wise interaction energy. It can be concluded that this derivative of Dansyl chloride with inherent high fluorescence intensity is a suitable reagent for the selective determination of the Er 3+ ion which can be used in constructing selective Er 3+ sensors.

Method to synthesize metal chalcogenide monolayer nanomaterials

Science.gov (United States)

Hernandez-Sanchez, Bernadette A.; Boyle, Timothy J.

2016-12-13

Metal chalcogenide monolayer nanomaterials can be synthesized from metal alkoxide precursors by solution precipitation or solvothermal processing. The synthesis routes are more scalable, less complex and easier to implement than other synthesis routes.

Syntheses, crystal structures and properties of novel copper(II) complexes obtained by reactions of copper(II) sulfate pentahydrate with tripodal ligands.

Science.gov (United States)

Zhao, Wei; Fan, Jian; Song, You; Kawaguchi, Hiroyuki; Okamura, Taka-aki; Sun, Wei-Yin; Ueyama, Norikazu

2005-04-21

Three novel metal-organic frameworks (MOFs), [Cu(1)SO4].H2O (4), [Cu2(2)2(SO4)2].4H2O (5) and [Cu(3)(H2O)]SO4.5.5H2O (6), were obtained by hydrothermal reactions of CuSO4.5H2O with the corresponding ligands, which have different flexibility. The structures of the synthesized complexes were determined by single-crystal X-ray diffraction analyses. Complex 4 has a 2D network structure with two types of metallacycles. Complex 5 also has a 2D network structure in which each independent 2D sheet contains two sub-layers bridged by oxygen atoms of the sulfate anions. Complex 6 has a 2D puckered structure in which the sulfate anions serve as counter anions, which are different from those in complexes 4 (terminators) and 5 (bridges). The different structures of complexes 4, 5 and 6 indicate that the nature of organic ligands affected the structures of the assemblies greatly. The magnetic behavior of complex 5 and anion-exchange properties of complex 6 were investigated.

15-00437_SI.doc

Indian Academy of Sciences (India)

2(NO3)3] (black) and (B)Nd(NO3)3.6H2O (red) & [ Nd(BPBH)2(NO3)3] (black ). in the visible region. 3. Table S1. Colors, analytical data, molar conductivities and Melting points of the BPBH ligand and. its Lanthanide(III) complexes. 4. Table S2.

Syntheses, structures and characterizations of three novel vanadium selenites with organically bonded copper/nickel complex

International Nuclear Information System (INIS)

Qian, Cheng; Kong, Fang; Mao, Jiang-Gao

2016-01-01

A series of vanadium selenites covalently bonded with metal-organic complex, namely, Ni(2,2-bipy) 2 V 2 O 4 (SeO 3 ) 2 (1), Cu(2,2-bipy)V 2 O 4 (SeO 3 ) 2 ·0.5H 2 O (2) and Cu 2 (2,2-bipy) 2 V 5 O 12 (SeO 3 ) 2 (3) (2,2-bipy=2,2-bipyridine) have been hydrothermally synthesized and structurally characterized. They exhibit three different structural dimensions, from 0D cluster, 1D chain to 2D layer. Compound 1 features a 0D {Ni(2,2-bipy) 2 V 2 O 4 (SeO 3 ) 2 } 2 dimeric cluster composed of two {Ni(2,2-bipy) 2 } 2+ moieties connected by the {V 4 O 8 (SeO 3 ) 4 } 4- cluster. Compound 2 shows a 1D {Cu(2,2-bipy)V 2 O 4 (SeO 3 ) 2 } n chain in which the {Cu 2 (2,2-bipy) 2 } 4+ moieties are bridged by the {V 4 O 8 (SeO 3 ) 4 } 4− clusters. Compound 3 displays a 2D structure consisted of mixed valence vanadium selenites layers {V IV V V 4 Se IV 2 O 18 } n 4− and {Cu(2,2-bipy)} 2+ complex moieties. The adjacent layers are further interconnected via π-π interactions between the 2,2-bipy ligands exhibiting an interesting 3D supramolecular architecture. Both compound 1 and 2 contain a new {V 4 O 8 (SeO 3 ) 4 } 4− cluster and compound 3 exhibits the first 2D vanadate polyhedral layer in vanadium selenites/tellurites with organic moieties. - Graphical abstract: We got three new vanadium selenites with organically linked copper/nickel complex, namely, Ni(2,2-bipy) 2 V 2 O 4 (SeO 3 ) 2 (1), Cu(2,2-bipy)V 2 O 4 (SeO 3 ) 2 ·0.5H 2 O (2) and Cu 2 (2,2-bipy) 2 V 5 O 12 (SeO 3 ) 2 (3) by hydrothermally syntheses. They display three different structural dimensions, from 0D cluster, to 1D chain and 2D layer. Display Omitted - Highlights: • Three new compounds display three different structural dimensions, from 0D cluster, to 1D chain and 2D layer. • The Tetranuclear {V 4 O 8 (SeO 3 ) 4 } 4− cluster and the vanadate {V 5 O 17 } n 2D layer are observed firstly. • Optical Properties and Magnetic Properties of three compounds are reported.

Construction of Polynuclear Lanthanide (Ln = Dy(III), Tb(III), and Nd(III)) Cage Complexes Using Pyridine-Pyrazole-Based Ligands: Versatile Molecular Topologies and SMM Behavior.

Science.gov (United States)

Bala, Sukhen; Sen Bishwas, Mousumi; Pramanik, Bhaskar; Khanra, Sumit; Fromm, Katharina M; Poddar, Pankaj; Mondal, Raju

2015-09-08

Employment of two different pyridyl-pyrazolyl-based ligands afforded three octanuclear lanthanide(III) (Ln = Dy, Tb) cage compounds and one hexanuclear neodymium(III) coordination cage, exhibiting versatile molecular architectures including a butterfly core. Relatively less common semirigid pyridyl-pyrazolyl-based asymmetric ligand systems show an interesting trend of forming polynuclear lanthanide cage complexes with different coordination environments around the metal centers. It is noteworthy here that construction of lanthanide complex itself is a challenging task in a ligand system as soft N-donor rich as pyridyl-pyrazol. We report herein some lanthanide complexes using ligand containing only one or two O-donors compare to five N-coordinating sites. The resultant multinuclear lanthanide complexes show interesting magnetic and spectroscopic features originating from different spatial arrangements of the metal ions. Alternating current (ac) susceptibility measurements of the two dysprosium complexes display frequency- and temperature-dependent out-of-phase signals in zero and 0.5 T direct current field, a typical characteristic feature of single-molecule magnet (SMM) behavior, indicating different energy reversal barriers due to different molecular topologies. Another aspect of this work is the occurrence of the not-so-common SMM behavior of the terbium complex, further confirmed by ac susceptibility measurement.

Creation, synthesis and characterisation of nitrogenous poly-heterocyclic new molecules for specific complexation of metallic cations; Conception, synthese et caracterisation de molecules polyheterocycliques azotees pour la complexation specifique de cations metalliques

Energy Technology Data Exchange (ETDEWEB)

Dupont, C.

2010-12-10

In France, the nuclear waste issued from the industrial reprocessing of spent nuclear fuels (by the PUREX process) are currently vitrified at the La Hague plant, waiting for a final disposal in a deep geological repository. The law voted in June 2006 on the management of highly active nuclear waste plans to look for solutions enabling the separation and transmutation of long-lived radionuclides so as to reduce the quantity and noxiousness of the final nuclear waste. To address this issue, the CEA investigates and elaborates advanced separation processes based on specially designed complexing or extracting molecules to selectively extract minor actinides from PUREX raffinates containing fission products like lanthanides, which are neutron scavengers. BTP or bis-triazinyl-pyridines have been extensively studied at the CEA (and in Europe) for actinides(III)/lanthanides(III) separation. They complex actinides(III) selectively. However, they are sensitive to degradation by hydrolysis and radiolysis. Besides, their separation mechanisms are not well understood, especially the influence of their substituting groups on their complexing and extracting properties. The first part of work reports the syntheses of various BTP and BTBP molecules, differently substituted, as well as a new family of poly-aromatic nitrogen-contained ligands: BPBT, presenting a pyridine/triazine sequence that has never been reported in the literature. The second part is devoted to the physico-chemistry studies of the synthesized molecules, such as the determination of their protonation and complexation constants to describe the influence of different substituting groups. Finally, the last part outlines solvent extraction studies by using these ligands either like extractants or like complexants. (author) [French] Resume: La loi du 6 juin 2006 sur la gestion des dechets radioactifs de haute activite et a vie longue prevoit la recherche de solutions permettant la separation et la transmutation des

Optical imaging of localized chemical events using programmable diamond quantum nanosensors

Czech Academy of Sciences Publication Activity Database

Rendler, T.; Neburková, Jitka; Zemek, O.; Kotek, J.; Zappe, A.; Chu, Z.; Cígler, Petr; Wrachtrup, J.

2017-01-01

Roč. 8, Mar 20 (2017), č. článku 14701. ISSN 2041-1723 R&D Projects: GA ČR(CZ) GA16-16336S Institutional support: RVO:61388963 Keywords : fluorescent nanodiamonds * lanthanide(III) complexes * ambient conditions Subject RIV: BO - Biophysics OBOR OECD: Biophysics Impact factor: 12.124, year: 2016 https://www.nature.com/articles/ncomms14701

Lanthanum-doped mesostructured strontium titanates synthesized via sol–gel combustion route using citric acid as complexing agent

Energy Technology Data Exchange (ETDEWEB)

Sukpanish, Polthep [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Patumwan, Bangkok 10330 (Thailand); Center of Excellence on Petrochemical and Materials Technology (PETROMAT), Chulalongkorn University, Patumwan, Bangkok 10330 (Thailand); Lertpanyapornchai, Boontawee [Program in Petrochemistry, Faculty of Science, Chulalongkorn University, Patumwan, Bangkok 10330 (Thailand); Yokoi, Toshiyuki [Division of Catalytic Chemistry, Chemical Resources Laboratory, Tokyo Institute of Technology, 4259 Nagatsuta, Midori-ku, Yokohama 226-8503 (Japan); Ngamcharussrivichai, Chawalit, E-mail: Chawalit.Ng@chula.ac.th [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Patumwan, Bangkok 10330 (Thailand); Center of Excellence on Petrochemical and Materials Technology (PETROMAT), Chulalongkorn University, Patumwan, Bangkok 10330 (Thailand)

2016-09-15

In the present work, a series of lanthanum-doped mesostructured strontium titanate (LMST) materials with different La/Sr ratios were synthesized via a sol–gel combustion method in the presence of citric acid as a complexing agent and Pluronic P123 as a templating agent. The effects of the amount of doped La and calcination temperature on the physicochemical properties of the LMSTs were examined using various techniques. Powder X-ray diffraction confirmed the substitution of La{sup 3+} into the SrTiO{sub 3} lattice, generating cubic perovskite La{sub x}Sr{sub 1−x}TiO{sub 3}, for the LMST materials calcined at 600 °C. The purity and crystallinity of the desired perovskite phase were enhanced by citric acid addition. The solubility limit of La{sup 3+} substitution at an La/Sr ratio of 0.43 was determined by structural and morphological studies. Increasing the La doping amount decreased the crystallinity and compositional homogeneity, because an La-rich amorphous phase segregated on the surface, but improved the mesoporosity. N{sub 2} physisorption measurements indicated that the LMSTs had a bimodal pore size distribution, of which the larger one was characterized by the crystallite size of mixed oxides, and the specific surface area of 24.9–37.3 m{sup 2} g{sup −1}. The formation of mesopores in the LMST materials synthesized via sol–gel combustion was explained based on a combination of soft- and hard-templating chemistries. - Highlights: • La-doped mesoporous SrTiO{sub 3} (LMST) was prepared first time via sol-gel combustion. • Pluronic P123 triblock copolymer was used as a cheap templating agent. • Citric acid as a complexing agent enhanced the purity and crystallinity of SrTiO{sub 3}. • The textural properties of LMST were improved by increasing the La doping amount. • Mesopore formation was explained by a combined soft- and hard-templating route.

Spectral characterization and DNA binding properties of lanthanide(III)

African Journals Online (AJOL)

Spectral data of complexes suggest that the ligand binds metal ion through pyridine- nitrogen, azomethine-nitrogen and amido-oxygen donor atoms. Electrochemical behaviour of metal complexes was investigated by using cyclic voltammetry. The complexes undergo quasi-reversible one electron reduction. The binding ...

Cyanide bridged hetero-metallic polymeric complexes: Syntheses, vibrational spectra, thermal analyses and crystal structures of complexes [M(1,2-dmi)2Ni(μ-CN)4]n (M = Zn(II) and Cd(II))

Science.gov (United States)

Kürkçüoğlu, Güneş Süheyla; Sayın, Elvan; Şahin, Onur

2015-12-01

Two cyanide bridged hetero-metallic complexes of general formula, [M(1,2-dmi)2Ni(μ-CN)4]n (1,2-dmi = 1,2-dimethylimidazole and M = Zn(II) or Cd(II)) have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal analyses and elemental analyses. The crystallographic analyses reveal that the complexes, [Zn(1,2-dmi)2Ni(μ-CN)4] (1) and [Cd(1,2-dmi)2Ni(μ-CN)4] (2), have polymeric 2D networks. In the complexes, four cyanide groups of [Ni(CN)4]2- coordinated to the adjacent M(II) ions and distorted octahedral geometries of complexes are completed by two nitrogen atoms of trans 1,2-dmi ligands. The structures of 1 and 2 are similar and linked via intermolecular hydrogen bonding, C-H⋯Ni interactions to give rise to 3D networks. Vibration assignments are given for all the observed bands and the spectral features also supported to the crystal structures of heteronuclear complexes. The FT-IR and Raman spectra of the complexes are very much consistent with the structural data presented.

The Mini-Chromosome Maintenance (Mcm) Complexes Interact with DNA Polymerase α-Primase and Stimulate Its Ability to Synthesize RNA Primers

Science.gov (United States)

You, Zhiying; De Falco, Mariarosaria; Kamada, Katsuhiko; Pisani, Francesca M.; Masai, Hisao

2013-01-01

The Mini-chromosome maintenance (Mcm) proteins are essential as central components for the DNA unwinding machinery during eukaryotic DNA replication. DNA primase activity is required at the DNA replication fork to synthesize short RNA primers for DNA chain elongation on the lagging strand. Although direct physical and functional interactions between helicase and primase have been known in many prokaryotic and viral systems, potential interactions between helicase and primase have not been explored in eukaryotes. Using purified Mcm and DNA primase complexes, a direct physical interaction is detected in pull-down assays between the Mcm2∼7 complex and the hetero-dimeric DNA primase composed of the p48 and p58 subunits. The Mcm4/6/7 complex co-sediments with the primase and the DNA polymerase α-primase complex in glycerol gradient centrifugation and forms a Mcm4/6/7-primase-DNA ternary complex in gel-shift assays. Both the Mcm4/6/7 and Mcm2∼7 complexes stimulate RNA primer synthesis by DNA primase in vitro. However, primase inhibits the Mcm4/6/7 helicase activity and this inhibition is abolished by the addition of competitor DNA. In contrast, the ATP hydrolysis activity of Mcm4/6/7 complex is not affected by primase. Mcm and primase proteins mutually stimulate their DNA-binding activities. Our findings indicate that a direct physical interaction between primase and Mcm proteins may facilitate priming reaction by the former protein, suggesting that efficient DNA synthesis through helicase-primase interactions may be conserved in eukaryotic chromosomes. PMID:23977294

The mini-chromosome maintenance (Mcm complexes interact with DNA polymerase α-primase and stimulate its ability to synthesize RNA primers.

Directory of Open Access Journals (Sweden)

Zhiying You

Full Text Available The Mini-chromosome maintenance (Mcm proteins are essential as central components for the DNA unwinding machinery during eukaryotic DNA replication. DNA primase activity is required at the DNA replication fork to synthesize short RNA primers for DNA chain elongation on the lagging strand. Although direct physical and functional interactions between helicase and primase have been known in many prokaryotic and viral systems, potential interactions between helicase and primase have not been explored in eukaryotes. Using purified Mcm and DNA primase complexes, a direct physical interaction is detected in pull-down assays between the Mcm2~7 complex and the hetero-dimeric DNA primase composed of the p48 and p58 subunits. The Mcm4/6/7 complex co-sediments with the primase and the DNA polymerase α-primase complex in glycerol gradient centrifugation and forms a Mcm4/6/7-primase-DNA ternary complex in gel-shift assays. Both the Mcm4/6/7 and Mcm2~7 complexes stimulate RNA primer synthesis by DNA primase in vitro. However, primase inhibits the Mcm4/6/7 helicase activity and this inhibition is abolished by the addition of competitor DNA. In contrast, the ATP hydrolysis activity of Mcm4/6/7 complex is not affected by primase. Mcm and primase proteins mutually stimulate their DNA-binding activities. Our findings indicate that a direct physical interaction between primase and Mcm proteins may facilitate priming reaction by the former protein, suggesting that efficient DNA synthesis through helicase-primase interactions may be conserved in eukaryotic chromosomes.

(II) complexes

African Journals Online (AJOL)

activities of Schiff base tin (II) complexes. Neelofar1 ... Conclusion: All synthesized Schiff bases and their Tin (II) complexes showed high antimicrobial and ...... Singh HL. Synthesis and characterization of tin (II) complexes of fluorinated Schiff bases derived from amino acids. Spectrochim Acta Part A: Molec Biomolec.

Syntheses, structures and characterizations of three novel vanadium selenites with organically bonded copper/nickel complex

Energy Technology Data Exchange (ETDEWEB)

Qian, Cheng [College of Chemistry, Fuzhou University, Fuzhou, Fujian 350002 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Kong, Fang [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Mao, Jiang-Gao, E-mail: mjg@fjirsm.ac.cn [College of Chemistry, Fuzhou University, Fuzhou, Fujian 350002 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China)

2016-06-15

A series of vanadium selenites covalently bonded with metal-organic complex, namely, Ni(2,2-bipy){sub 2}V{sub 2}O{sub 4}(SeO{sub 3}){sub 2} (1), Cu(2,2-bipy)V{sub 2}O{sub 4}(SeO{sub 3}){sub 2}·0.5H{sub 2}O (2) and Cu{sub 2}(2,2-bipy){sub 2}V{sub 5}O{sub 12}(SeO{sub 3}){sub 2} (3) (2,2-bipy=2,2-bipyridine) have been hydrothermally synthesized and structurally characterized. They exhibit three different structural dimensions, from 0D cluster, 1D chain to 2D layer. Compound 1 features a 0D {Ni(2,2-bipy)_2V_2O_4(SeO_3)_2}{sub 2} dimeric cluster composed of two {Ni(2,2-bipy)_2}{sup 2+} moieties connected by the {V_4O_8(SeO_3)_4}{sup 4-} cluster. Compound 2 shows a 1D {Cu(2,2-bipy)V_2O_4(SeO_3)_2}{sub n} chain in which the {Cu_2(2,2-bipy)_2}{sup 4+} moieties are bridged by the {V_4O_8(SeO_3)_4}{sup 4−} clusters. Compound 3 displays a 2D structure consisted of mixed valence vanadium selenites layers {V"I"VV"V_4Se"I"V_2O_1_8}{sub n}{sup 4−} and {Cu(2,2-bipy)}{sup 2+} complex moieties. The adjacent layers are further interconnected via π-π interactions between the 2,2-bipy ligands exhibiting an interesting 3D supramolecular architecture. Both compound 1 and 2 contain a new {V_4O_8(SeO_3)_4}{sup 4−} cluster and compound 3 exhibits the first 2D vanadate polyhedral layer in vanadium selenites/tellurites with organic moieties. - Graphical abstract: We got three new vanadium selenites with organically linked copper/nickel complex, namely, Ni(2,2-bipy){sub 2}V{sub 2}O{sub 4}(SeO{sub 3}){sub 2} (1), Cu(2,2-bipy)V{sub 2}O{sub 4}(SeO{sub 3}){sub 2}·0.5H{sub 2}O (2) and Cu{sub 2}(2,2-bipy){sub 2}V{sub 5}O{sub 12}(SeO{sub 3}){sub 2} (3) by hydrothermally syntheses. They display three different structural dimensions, from 0D cluster, to 1D chain and 2D layer. Display Omitted - Highlights: • Three new compounds display three different structural dimensions, from 0D cluster, to 1D chain and 2D layer. • The Tetranuclear {V_4O_8(SeO_3)_4}{sup 4−} cluster and the vanadate {V

Widely tunable THz synthesizer

Science.gov (United States)

Hindle, F.; Mouret, G.; Eliet, S.; Guinet, M.; Cuisset, A.; Bocquet, R.; Yasui, T.; Rovera, D.

2011-09-01

The generation of cw-THz radiation by photomixing is particularly suited to the high resolution spectroscopy of gases; nevertheless, until recently, it has suffered from a lack of frequency metrology. Frequency combs are a powerful tool that can transfer microwave frequency standards to optical frequencies and a single comb has permitted accurate (10-8) THz frequency synthesis with a limited tuning range. A THz synthesizer composed of three extended cavity laser diodes phase locked to a frequency comb has been constructed and its utility for high resolution gas phase spectroscopy demonstrated. The third laser diode allows a larger tuning range of up to 300 MHz to be achieved without the need for large frequency excursions, while the frequency comb provides a versatile link to be established from any traceable microwave frequency standard. The use of a single frequency comb as a reference for all of the cw-lasers eliminates the dependency of synthesized frequency on the carrier envelope offset frequency. This greatly simplifies the frequency comb stabilization requirements and leads to a reduced instrument complexity.

Luminescence and Electronic Spectral Studies of Some Synthesized Lanthanide Complexes Using Benzoic Acid Derivative and o-Phenanthroline.

Science.gov (United States)

Wankar, Sneha; Limaye, S N

2015-07-01

Lanthanide complexes of p-nitrobenzoic acid(p-NBA) and o-phenanthroline(o-phen) namely [Ln2(Phen)2(p-NBA)3(NO3)2].2H2O where, Ln = Sm(III),Tb(III),Dy(III) and [Eu2(Phen)2(p-NBA)3].4H2O were synthesized and further characterized by Elemental analysis, UV spectroscopy, IR spectroscopy, (1)HNMR spectroscopy. Luminescence measurements were performed on all compounds in ethanolic solution. These complexes have showed narrow emission indicating that the organic ligands are better energy absorber and capable of transferring energy to the Ln (III) ion. Furthermore, we reported electronic spectral studies on [Eu2 (Phen)2 (p-NBA)3].4H2O in order to calculate following parameters, viz: Oscillator strength (f), Judd-Ofelt parameters Ωλ (λ = 2,4,6) and Radiative parameters. [Eu2 (o-Phen)2 (p-NBA)3].4H2O showed the strongest emission at 613 nm corresponds to (5)D0→(7)F2 hypersensitive transition, this emission is very sensitive to the environment. However, the larger value of Ω2 supports the presence of the hypersensitive transition (5)D0→(7)F2 which strictly depends on the nature of ligand. All electronic spectral parameters were calculated systemically.

Syntheses, spectroscopic properties and molecular structure of silver phytate complexes - IR, UV-VIS studies and DFT calculations

Science.gov (United States)

Zając, A.; Dymińska, L.; Lorenc, J.; Ptak, M.; Hanuza, J.

2018-03-01

Silver phytate IP6, IP6Ag, IP6Ag2 and IP6Ag3 complexes in the solid state have been synthesized changing the phosphate to metal mole ratio. The obtained products have been characterized by means of chemical and spectroscopic studies. Attenuated total reflection Fourier transform infrared technique and Raman microscope were used in the measurements. These results were discussed in terms of DFT (Density Functional Theory) quantum chemical calculations using the B3LYP/6-31G(d,p) approach. The molecular structures of these compounds have been proposed on the basis of group theory and geometry optimization taking into account the shape and the number of the observed bands corresponding to the stretching and bending vibrations of the phosphate group and metal-oxygen polyhedron. The role of inter- and intra-hydrogen bonds in stabilization of the structure has been discussed. It was found that three types of hydrogen bonds appear in the studied compounds: terminal, and those engaged in the inter- and intra-molecular interactions. The Fermi resonance as a result of the strong intra-molecular Osbnd H⋯O hydrogen bonds was discovered. Electron absorption spectra have been measured to characterize the electron properties of the studied complexes and their local symmetry.

Syntheses and spectroscopic properties of mercury(II) and nickel(II ...

African Journals Online (AJOL)

Syntheses and spectroscopic properties of mercury(II) and nickel(II) ... The complexes were characterized by IR, diffuse reflectance, 1H NMR spectra and elemental ... coordinating through thiolato sulphur and hydrazinic nitrogen atoms.

Investigation of synthesized new vanadium(III) complexes of ditolyldithiophosphate ligands by spectroscopic, cyclic voltammetric, DFT, antimicrobial and cytotoxic studies

Science.gov (United States)

Kumar, Sandeep; Syed, Atiya; Andotra, Savit; Kaur, Ramanpreet; Vikas; Pandey, Sushil K.

2018-02-01

Vanadium(III) complexes with sulfur donor dithiophosphate ligands corresponding to [{(ArO)2PS2}3V] and [{(ArO)2PS2}2VCl.L] (Ar = o-, m-, p-CH3C6H4 and p-Cl-m-CH3C6H3; L = NC5H5, P(C6H5)3, have been synthesized and characterized by various physico-chemical techniques like elemental analyses, magnetic studies, ESI-Mass, IR, UV and heteronuclear NMR (1H, 13C and 31P) spectral studies. These analyses have contributed to the prediction of structure: by exhibiting significant v(P-S) and v(Pdbnd S) band shifting in comparative IR spectra; shifting of resonance signal in comparative 31P NMR spectra of ligands and complexes and stability of V(III) ion in the complexed state is confirmed by magnetic and UV studies. Therefore, the six coordinated geometry stabilizing the trivalent vanadium atom in the complexes and adducts, respectively has been confirmed. The cyclic voltammetric analyses presented the redox aptitude of the complex under analysis which can be utilized as catalyst in organic synthesis. The geometry of ligands and complexes has been optimized using density functional theory (DFT). The structural parameters, vibrational bands and energy gaps of frontier orbitals (HOMO-LUMO) have also been calculated. The calculated geometric and spectral results reproduced the experimental data with well agreement. The DFT computed frontier molecular orbitals (HOMO-LUMO) and their energies suggest charge transfer occurs within the complexes. Antimicrobial screening of the complexes against two bacterial strains: Gram-positive, Enterrococcus faecalis and Gram-negative, Eischerichia coli and fungus Fusarium oxysporum have shown potential bioactivity. A preliminary cytotoxic analysis has been carried out using the cultivated human cell lines: lung adeno carcinoma cell line A-549, leukemia cell line THP-1, prostate cancer cell line PC3 and colorectal cancer cell line HCT-116.

Syntheses, structural characterization and spectroscopic studies of cadmium(II)-metal(II) cyanide complexes with 4-(2-aminoethyl)pyridine

Science.gov (United States)

Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Hökelek, Tuncer

2017-02-01

Three new cadmium(II)-metal(II) cyanide complexes, [Cd(4aepy)2(H2O)2][Ni(CN)4] (1), [Cd(4aepy)2(H2O)2][Pd(CN)4] (2) and [Cd(4aepy)2(H2O)2][Pt(CN)4] (3) [4aepy = 4-(2-aminoethyl)pyridine], have been synthesized and characterized by elemental, thermal, FT-IR and Raman spectral analyses. The crystal structures of 1 and 2 have been determined by single crystal X-ray diffraction technique, in which they crystallize in the monoclinic system and C2/c space group. The M(II) [M(II) = Ni(II), Pd(II) and Pt(II)] ions are coordinated with the carbon atoms of the four cyanide groups in the square planar geometries and the [M(CN)4]2- ions act as counter ions. The Cd(II) ions display an N4O2 coordination sphere with a distorted octahedral geometry, the nitrogen donors belonging to four molecules of the organic 4aepy that act as unidentate ligands and two oxygen atoms from aqua ligands. 3D supramolecular structures of 1 and 2 were occurred by M⋯π and hydrogen bonding (Nsbnd H⋯N and Osbnd H⋯N) interactions. Vibrational assignments of all the observed bands were given and the spectral properties were also supported the crystal structures of the complexes. A possible decompositions of the complexes were investigated in the temperature range 30-800 °C in the static atmosphere.

Lanthanide(III) complexes with μ-SnSe{sub 4} and μ-Sn{sub 2}Se{sub 6} linkers. Solvothermal syntheses and properties of new Ln(III) selenidostannates decorated with linear polyamine

Energy Technology Data Exchange (ETDEWEB)

Liu, Shuzhen; Sun, Peipei; Shen, Yali; Han, Jingyu; Sun, Hui; Jia, Dingxian [Soochow Univ., Suzhou (China). College of Chemistry, Chemical Engineering and Materials Science

2017-06-01

New lanthanide-selenidostannate complexes [{La(peha)(Cl)}{La(peha)(NO_3)}(μ-1κ{sup 2}:2κ{sup 2}-SnSe{sub 4})] (1), [H{sub 2}trien][{La(trien)_2}{sub 2}(μ-1-κ:2κ-Sn{sub 2}Se{sub 6})][Sn{sub 2}Se{sub 6}].H{sub 2}O (2) and [{Ln(tepa)(μ-OH)}{sub 2}(μ-1κ:2κ-Sn{sub 2}Se{sub 6})]{sub n}.nH{sub 2}O (Ln=Sm(3), Eu(4)) were prepared by solvothermal methods in pentaethylenehexamine (peha), triethylenetetramine (trien) and tetraethylenepentamine (tepa), respectively. Acting as a tetradentate chelating and bridging ligand, μ-1κ{sup 2}:2κ{sup 2}-SnSe{sub 4}, the tetrahedral SnSe{sub 4} unit joins {La(peha)(Cl)}{sup 2+} and {La(peha)(NO_3)}{sup 2+} complex fragments to generate the neutral coordination compound 1. The tetradentate μ-1κ{sup 2}:2κ{sup 2} bridge in 1 represents a new coordination mode for the SnSe{sub 4} tetrahedron. In 2, dinuclear [Sn{sub 2}Se{sub 6}]{sup 4-} anions are formed of SnSe{sub 4} tetrahedra via edge-sharing. One [Sn{sub 2}Se{sub 6}]{sup 4-} anion acts as a bidentate bridging ligand in a μ-1κ:2κ coordination mode to join two {La(trien)_2}{sup 3+} units, and the other [Sn{sub 2}Se{sub 6}]{sup 4-} anion exists as a free charge compensating ion. In 3 and 4, the [Sn{sub 2}Se{sub 6}]{sup 4-} anion connects binuclear [{Ln(tepa)(μ-OH)}{sub 2}]{sup 2+}(Ln=Sm, Eu) units with a bidentate μ-1κ:2κ mode, giving neutral coordination polymers [{Ln(tepa)(μ-OH)}{sub 2}(μ-1κ:2κ-Sn{sub 2}Se{sub 6})]{sub n}. The La(2){sup 3+} ion in 1 is in a 10-fold coordination environment of LaN{sub 6}O{sub 2}Se{sub 2}, whereas the La(1){sup 3+} ions in 1 and 2 are in 9-fold coordinated environments forming polyhedra LaN{sub 6}ClSe{sub 2} and LaN{sub 8}Se, respectively. The Sm{sup 3+} and Eu{sup 3+} ions in 3 and 4 are both in an 8-fold coordination environment of LnN{sub 5}O{sub 2}Se. Compounds 1-4 exhibit optical band gaps between 2.21 and 2.42 eV. Their thermal stabilities were investigated by thermogravimetric analyses.

Syntheses of 2-nitroimidazole derivatives conjugated with 1,4,7-triazacyclononane-N,N'-diacetic acid labeled with F-18 using an aluminum complex method for hypoxia imaging.

Science.gov (United States)

Hoigebazar, Lathika; Jeong, Jae Min; Lee, Ji-Youn; Shetty, Dinesh; Yang, Bo Yeun; Lee, Yun-Sang; Lee, Dong Soo; Chung, June-Key; Lee, Myung Chul

2012-04-12

Hypoxia imaging is important for diagnosis of ischemic diseases, and thus various (18)F-labeled radiopharmaceuticals have been developed. However, (18)F-labeling requires multistep procedures including azeotropic distillation, which is complicated and difficult to automate. Recently, (18)F-labeling method using Al-F complex in aqueous solution was devised that offered a straightforward (18)F-labeling procedure. We synthesized nitroimidazole derivatives conjugated with 1,4,7-triazacyclononane-1,4-diacetic acid (NODA) that can be labeled with (18)F using Al-F complex and examined their radiochemistries, in vitro and in vivo biological properties, and animal PET imaging characteristics. We found that the synthesized derivatives have excellent (18)F-labeling efficiencies, high stabilities, specific uptakes in cultured hypoxic tumor cells, and high tumor to nontumor ratios in xenografted mice. Furthermore, the derivatives were labeled with (18)F in a straightforward manner within 15 min at high labeling efficiencies and radiochemical purities. In conclusion, (18)F-labeled NODA-nitroimidazole conjugates were developed and proved to be promising hypoxia PET agents. © 2012 American Chemical Society

Uranium and lanthanide complexes with the 2-mercapto benzothiazolate ligand: Evidence for a specific covalent binding site in the differentiation of isostructural lanthanide(III) and actinide(III) compounds

Energy Technology Data Exchange (ETDEWEB)

Roger, M.; Arliguie, T.; Thuery, P.; Ephritikhine, M. [CEA Saclay, DSM, DRECAM, Serv Chim Mol, CNRS URA 331, F-91191 Gif Sur Yvette, (France); Belkhiri, L. [Univ Mentouri Constantine, Fac Sci, Dept Chim, Lab Chim Mol LACMOM, Constantine 25017, (Algeria); Boucekkine, A. [Univ Rennes 1, CNRS, UMR Sci Chim Rennes 6226, F-35042 Rennes, (France)

2008-07-01

Treatment Of [U(Cp*){sub 2}Cl{sub 2}] with KSBT in THF gave [U(Cp*){sub 2}(SBT){sub 2}], which exhibits the usual bent sandwich configuration in the solid state with the two SBT ligands adopting the bidentate ligation mode. The mono-cyclopentadienyl compound [U(Cp*)(SBT){sub 3}] was synthesized by reaction of [U(Cp*)(BH{sub 4}){sub 3}] with KSBT in THF, and its reduction with potassium amalgam in the presence of 18-crown-6 afforded the corresponding anionic complex [K(18-crown-6)(THF){sub 2}][U(Cp*)(SBT){sub 3}]. The lanthanide analogues [K(THF){sub 2}Ln(Cp*)(SBT){sub 3}] were obtained by treating [Ln(BH{sub 4}){sub 3}(THF){sub 3}] with KSBT and KCp*; isomorphous crystals of [K(15-crown-5){sub 2}] [Ln(Cp*)(SBT){sub 3}].THF [Ln = La, Ce, Nd] were formed upon addition of 15-crown-5. Comparison of the crystal structures of the pentagonal bipyramidal complexes [M(Cp*)(SBT){sub 3}]{sup -} reveals that the M-Nax distances are shorter than the M-Neq distances, whatever the metal, the phenomenon being enhanced in the U(III) compound versus the Ln(III) analogues. The structural data obtained by relativistic density functional theory (DFT) calculations reproduce experimental trends. Electronic population and molecular orbital analyses show that the structural differences in the series of [M(Cp*)(SBT){sub 3}]{sup -} anions are related to the uranium 5f orbital-ligand mixing, which is greater than the lanthanide 4f orbital-ligand mixing. Moreover, the consideration of the corresponding bond orders and the analysis of the bonding energy bring to light a strong and specific interaction between the uranium and apical nitrogen atoms. (authors)

An Open-Source Automated Peptide Synthesizer Based on Arduino and Python.

Science.gov (United States)

Gali, Hariprasad

2017-10-01

The development of the first open-source automated peptide synthesizer, PepSy, using Arduino UNO and readily available components is reported. PepSy was primarily designed to synthesize small peptides in a relatively small scale (<100 µmol). Scripts to operate PepSy in a fully automatic or manual mode were written in Python. Fully automatic script includes functions to carry out resin swelling, resin washing, single coupling, double coupling, Fmoc deprotection, ivDde deprotection, on-resin oxidation, end capping, and amino acid/reagent line cleaning. Several small peptides and peptide conjugates were successfully synthesized on PepSy with reasonably good yields and purity depending on the complexity of the peptide.

Structural characterization of the Actinides (III) and (IV) - DOTA complexes

International Nuclear Information System (INIS)

Audras, Matthieu

2014-01-01

The polyamino-carboxylate anions have been identified as compounds of interest in the operations of actinide separation, in actinide migration in the environment and in human radio-toxicology. The structural characterization of complexes formed between actinides and polyamino-carboxylates ligands is essential for a better understanding of actinide-ligands interactions. Among the polyamino-carboxylate anions, the DOTA ligand (1,4,7,10-tetraaza-cyclododecane tetraacetic acid) is described as a very strong complexing agent of the lanthanides(III), but has been little studied with actinides. The objective of this thesis is to describe the complexes formed between the actinides (III) and (IV) and the DOTA ligand, and compare them with the lanthanide complexes. For this, an approach has been introduced to characterize the complexes by complementary analytical techniques (spectrophotometry, electro-spray ionization mass spectrometry, NMR, EXAFS, electrochemistry), but also by calculations of theoretical chemistry to help the interpretation of the experimental data. The formation of a 1:1 complex is observed with the actinides(III) (plutonium and americium) as for lanthanides(III): rapid formation of intermediate species which evolves slowly towards the formation of a limit complex. Within this complex, the cation is located inside the cavity formed by the ligand. Four nitrogen atoms and four oxygen atoms from the carboxylate functions are involved in the coordination sphere of the cation. However, differences were observed in the bond lengths formed between the cation and the nitrogen atoms (the bonds are somewhat shorter in the case of actinide complexes) as well as the complexation kinetics, which is slightly faster for the actinides(III) than for lanthanide(III) ions of equivalent radius. The same behavior was observed in solution upon complexation of actinides(IV) (uranium, plutonium and neptunium): slow formation of a 1:1 complex (actinide(IV):ligand) in wherein the

Syntheses, structures and characterizations of three novel vanadium selenites with organically bonded copper/nickel complex

Science.gov (United States)

Qian, Cheng; Kong, Fang; Mao, Jiang-Gao

2016-06-01

A series of vanadium selenites covalently bonded with metal-organic complex, namely, Ni(2,2-bipy)2V2O4(SeO3)2 (1), Cu(2,2-bipy)V2O4(SeO3)2·0.5H2O (2) and Cu2(2,2-bipy)2V5O12(SeO3)2 (3) (2,2-bipy=2,2-bipyridine) have been hydrothermally synthesized and structurally characterized. They exhibit three different structural dimensions, from 0D cluster, 1D chain to 2D layer. Compound 1 features a 0D {Ni(2,2-bipy)2V2O4(SeO3)2}2 dimeric cluster composed of two {Ni(2,2-bipy)2}2+ moieties connected by the {V4O8(SeO3)4}4- cluster. Compound 2 shows a 1D {Cu(2,2-bipy)V2O4(SeO3)2}n chain in which the {Cu2(2,2-bipy)2}4+ moieties are bridged by the {V4O8(SeO3)4}4- clusters. Compound 3 displays a 2D structure consisted of mixed valence vanadium selenites layers {VIVVV4SeIV2O18}n4- and {Cu(2,2-bipy)}2+ complex moieties. The adjacent layers are further interconnected via π-π interactions between the 2,2-bipy ligands exhibiting an interesting 3D supramolecular architecture. Both compound 1 and 2 contain a new {V4O8(SeO3)4}4- cluster and compound 3 exhibits the first 2D vanadate polyhedral layer in vanadium selenites/tellurites with organic moieties.

The crystalline and magnetic properties of Zn doped strontium Z-type hexaferrite synthesized by polymerizable complex method

Directory of Open Access Journals (Sweden)

Jung Tae Lim

2017-05-01

Full Text Available Polycrystalline samples of Sr3Co2-xZnxFe24O41 (x = 0.0, 0.5, 1.0, 1.5, 2.0 were synthesized by a polymerizable complex method. The crystallographic, and magnetic properties of samples were investigated using x-ray diffractometer (XRD, vibrating sample magnetometer (VSM, and Mössbauer spectroscopy. The crystal structures of all samples were determined to be hexagonal with the space group P63/mmc. The hysteresis curves under 10 kOe at 295 K showed that all samples were not saturated due to the high planar anisotropy of Sr ions. In addition, the coercivity (Hc of samples decreased with increasing Zn ion contents. Mössbauer spectra of all samples were obtained at 295 K, and least-squares fitted below TC as six distinguishable sextets (4fIV, 4fIV*, 12kVI*, 4fVI*+ 4eIV, 12kVI, and 2dV + 2aVI + 4fVI + 4eVI.

Application of rank annihilation factor analysis to the spectrophotometric determination of the formation constant of complex of a new synthesized tripodal ligand with Co2+

Directory of Open Access Journals (Sweden)

Reza Golbedaghi

2017-05-01

Full Text Available The complex formation between a new synthesized tripodal ligand (L22py and the cation Co2+ in water was studied spectrophotometrically using rank annihilation factor analysis (RAFA. According to molar ratio data the stoichiometry of complexation between the ligand and the cation Co2+ was 1:1. Formation constant of this complex was derived using RAFA on spectrophotometric data. In this process the contribution of ligand is removed from the absorbance data matrix when the complex stability constant acts as an optimizing object and simply combined with the pure spectrum of ligand, the rank of original data matrix can be reduced by one by annihilating the information of the ligand from the original data matrix. The effect of ethanol, dimethylformamide (DMF and acetonitrile (AN was investigated on the formation constant of the Co2+ complex. Complex formation constant in water was estimated as log Kf = 5.09 ± 0.02. In mixtures of solvents of water and DMF and water and AN, the formation constant of the complex was increased because of lowering donor number of the solvent and in mixture of water and ethanol, the complex formation constant was decreased because of lowering of dielectric constant of the solvent.

Some high coordination compounds of lanthanides(III derived from N-isonicotinamidosalicyaldimine

Directory of Open Access Journals (Sweden)

Ram K. Agarwal

2000-12-01

Full Text Available A new series of lanthanide(III nitrates, isothiocyanates and perchlorates coordination complexes of N-isonicotinamidosalicyaldimine (INH-SAL with the general composition LnX3.n(INH-SAL (Ln = La, Pr, Nd, Sm, Gd, Tb or Dy; X = NO3-, n = 2; X = NCS-, n = 2 or 3 and X = ClO4-, n = 4 have been reported. All the complexes were characterized by chemical analyses, conductance, molar weight, magnetic moment measurements, infrared and electronic spectra. IR spectra indicate that the ligand behaves as a neutral N,O-donors. Thermal properties of the complexes have also been studied.

Writing syntheses for managers: Lessons from the Rainbow Series and Fire Effects Information System

Science.gov (United States)

Jane Kapler Smith; Kristin L. Zouhar; Janet Fryer

2009-01-01

Scientific knowledge is essential for sound wildland management, but this knowledge is a complex, ever-expanding resource. Managers often request syntheses or reviews of available knowledge, and scientists have responded with an increasing number of syntheses for managers. Unfortunately, little guidance is available for this kind of writing. While most scientists have...

A Two-Stage Approach to Synthesizing Covariance Matrices in Meta-Analytic Structural Equation Modeling

Science.gov (United States)

Cheung, Mike W. L.; Chan, Wai

2009-01-01

Structural equation modeling (SEM) is widely used as a statistical framework to test complex models in behavioral and social sciences. When the number of publications increases, there is a need to systematically synthesize them. Methodology of synthesizing findings in the context of SEM is known as meta-analytic SEM (MASEM). Although correlation…

Photocytotoxicity and DNA photocleavage activity of La(III) and Gd(III) complexes of phenanthroline bases

International Nuclear Information System (INIS)

Hussain, Akhtar; Saha, Sounik; Chakravarty, Akhil R.; Majumdar, Ritankar; Dighe, Rajan R.

2011-01-01

Lanthanide(III) complexes (La(B)(acac) 3 ) (1-3) and (Gd(B)(acac) 3 ) (4-6), where B is a N,N-donor phenanthroline base, viz., 1,10-phenanthroline (phen in 1, 4), dipyrido(3,2-d:2',3'-f)quinoxaline (dpq in 2, 5) and dipyrido(3,2-a:2',3'-c)phena-zine (dppz in 3, 6), have been prepared and characterized. The Gd(III) complexes 4 - 6 are structurally characterized by single crystal X-ray crystallography. The complexes display GdO 6 N 2 coordination with the ligands showing bidentate chelating mode of bonding. The complexes are non-electrolytic in aqueous DMF and exhibit ligand-centered absorption bands in the UV region. The dppz complexes show a band at 380 nm in DMF. The La(III) complexes are diamagnetic. The Gd(III) complexes are paramagnetic with magnetic moment that corresponds to seven unpaired electrons. The complexes are avid binders to calf thymus DNA giving K b values in the range of 4.7 x 10 4 - 6.1 x 10 5 M -1 with a relative binding order: 3, 6 (dppz) > 2, 5 (dpq) > 1, 4 (phen). The binding data suggest DNA surface and/or groove binding nature of the complexes. The dpq and dppz complexes efficiently cleave SC DNA to its nicked circular form in UV-A light of 365 nm via formation of both singlet oxygen ( 1 O 2 ) and hydroxyl radical (HO · ) species. The dppz complexes 3 and 6 exhibit significant PDT effect in HeLa cervical cancer cells giving respective IC 50 value of 460(±50) and 530(±30) nM in UV-A light of 365 nm, and are essentially non-toxic in dark with an IC 50 value of >100 μM. The dppz ligand alone is cytotoxic in dark and UV-A light. A significant decrease in the dark toxicity of the dppz base is observed on binding to the Ln(Ill) ion while retaining its photocytotoxicity. (author)

Rhenium complexes of chromophore-appended dipicolylamine ligands: syntheses, spectroscopic properties, DNA binding and X-ray crystal structure

International Nuclear Information System (INIS)

Mullice, L.A.; Buurma, N.J.; Pope, S.J.A.; Laye, R.H.; Harding, L.P.

2008-01-01

The syntheses of two chromophore-appended dipicolylamine-derived ligands and their reactivity with penta-carbonyl-chloro-rhenium have been studied. The resultant complexes each possess the fac-Re(CO) 3 core. The ligands L 1 1-[bis(pyridine-2-yl-methyl)amino]methyl-pyrene and L 2 2-[bis(pyridine-2-yl-methyl)amino]methyl-quinoxaline were isolated via a one-pot reductive amination in moderate yield. The corresponding rhenium complexes were isolated in good yields and characterised by 1 H NMR, MS, IR and UV-Vis studies. X-Ray crystallographic data were obtained for fac-{Re(CO) 3 (L 1 )}(BF 4 ), C 34 H 26 BF 4 N 4 O 3 Re: monoclinic, P2(1)/c, a 18.327(2) Angstroms, α = 90.00 degrees, b 14.1537(14) Angstroms, β96.263(6) degrees, c = 23.511(3) Angstroms, γ 90.00 Angstroms, 6062.4(11) (Angstroms) 3 , Z=8. The luminescence properties of the ligands and complexes were also investigated, with the emission attributed to the appended chromophore in each case. Isothermal titration calorimetry suggests that fac-{Re(CO) 3 (L 1 )}(BF 4 ) self-aggregates cooperatively in aqueous solution, probably forming micelle-like aggregates with a cmc of 0.18 mM. Investigations into the DNA-binding properties of fac-{Re(CO) 3 (L 1 )}(BF 4 ) were undertaken and revealed that fac-{Re(CO) 3 (L 1 )}(BF 4 ) binding to fish sperm DNA (binding constant 1.5 ± 0.2 * 10 5 M -1 , binding site size 3.2 ± 0.3 base pairs) is accompanied by changes in the UV-Vis spectrum as typically observed for pyrene-based intercalators while the calorimetrically determined binding enthalpy (-14 ± 2 kcal mol -1 ) also agrees favourably with values as typically found for intercalators. (authors)

Parametric Audio Based Decoder and Music Synthesizer for Mobile Applications

NARCIS (Netherlands)

Oomen, A.W.J.; Szczerba, M.Z.; Therssen, D.

2011-01-01

This paper reviews parametric audio coders and discusses novel technologies introduced in a low-complexity, low-power consumption audiodecoder and music synthesizer platform developed by the authors. Thedecoder uses parametric coding scheme based on the MPEG-4 Parametric Audio standard. In order to

Synthesis and characterisation of nitrogen-containing poly heterocyclic molecules for the complexation of polluting metal cations; Synthese et caracterisation de molecules polyheterocycliques azotees pour la complexation de cations metalliques polluants

Energy Technology Data Exchange (ETDEWEB)

Leconte, N

2007-12-15

The recovery of actinides(III) from the mixture actinides(III)/lanthanides(III) is a great deal of the nuclear waste management. Experiences have shown that derivatives of 2,6- bis(1,2,4-triazine-3-yl)pyridine (BTP) are able to extract selectively actinides(III) from lanthanides(III). But the properties of these molecules need to be reinforced to exhibit best extraction performances and to resist to the harsh conditions of the extracting processes. Originally functionalized ligands were synthesized and tested in a radioactive medium. In a second part, this work focuses on the control and the detection of actinides(III). This could be done thanks to the use of a chemical sensor such as quartz crystal microbalance. The study of this apparatus required the preliminary synthesis of original complexing BTP-derived structures. The last part of this work deals with the study of new synthetic ways to afford the BTP moiety. The palladium-catalyzed cross-coupling reaction of 3-methylthio-1,2,4-triazine with various 2-stannylated pyridines have been explored. Our investigations have also allowed to develop a method for synthesizing unsymmetrical 1,2,4,5-tetrazine from the cross-coupling reaction between 3-methylthio-6-(morpholine-N-yl)-1,2,4,5-tetrazine and organoboron / organo-stannane derivatives. (author)

Detection of Sugars via Chirality Induced in Europium(III) Compounds

Czech Academy of Sciences Publication Activity Database

Wu, Tao; Průša, Jiří; Kessler, Jiří; Dračínský, Martin; Valenta, J.; Bouř, Petr

2016-01-01

Roč. 88, č. 17 (2016), s. 8878-8885 ISSN 0003-2700 R&D Projects: GA ČR(CZ) GA16-05935S; GA ČR(CZ) GJ16-08764Y; GA ČR GA15-11223S; GA ČR GA15-09072S Institutional support: RVO:61388963 Keywords : Raman optical activity * molecular dynamics simulations * D-3 lanthanide(III) complexes Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 6.320, year: 2016

Structural, spectral and biological studies of binuclear tetradentate metal complexes of N 3O Schiff base ligand synthesized from 4,6-diacetylresorcinol and diethylenetriamine

Science.gov (United States)

Emara, Adel A. A.

2010-09-01

The binuclear Schiff base, H 2L, ligand was synthesized by reaction of 4,6-diacetylresorcinol with diethylenetriamine in the molar ratio 1:2. The coordination behavior of the H 2L towards Cu(II), Ni(II), Co(II), Zn(II), Fe(III), Cr(III), VO(IV) and UO 2(VI) ions has been investigated. The elemental analyses, magnetic moments, thermal studies and IR, electronic, 1H NMR, ESR and mass spectra were used to characterize the isolated ligand and its metal complexes. The ligand acts as dibasic with two N 3O-tetradentate sites and can coordinate with two metal ions to form binuclear complexes. The bonding sites are the nitrogen atoms of the azomethine and amine groups and the oxygen atoms of the phenolic groups. The metal complexes exhibit either square planar, tetrahedral, square pyramid or octahedral structures. The Schiff base ligand and its metal complexes were tested against four pathogenic bacteria ( Staphylococcus aureus and Streptococcus pyogenes) as Gram-positive bacteria, and ( Pseudomonas fluorescens and Pseudomonas phaseolicola) as Gram-negative bacteria and two pathogenic fungi ( Fusarium oxysporum and Aspergillus fumigatus) to assess their antimicrobial properties. Most of the complexes exhibit mild antibacterial and antifungal activities against these organisms.

Studies on the Alkaloids of the Calycanthaceae and Their Syntheses

Directory of Open Access Journals (Sweden)

Jin-Biao Xu

2015-04-01

Full Text Available Plants of the Calycanthaceae family, which possesses four genera and about 15 species, are mainly distributed in China, North America and Australia. Chemical studies on the Calycanthaceae have led to the discovery of about 14 alkaloids of different skeletons, including dimeric piperidinoquinoline, dimeric pyrrolidinoindoline and/or trimeric pyrrolidinoindolines, which exhibit significant anti-convulsant, anti-fungal, anti-viral analgesic, anti-tumor, and anti-melanogenesis activities. As some of complex tryptamine-derived alkaloids exhibit promising biological activities, the syntheses of these alkaloids have also been a topic of interest in synthetic chemistry during the last decades. This review will focus on the structures and total syntheses of these alkaloids.

Synthesis, spectroscopic characterization, solid state d.c. electrical conductivity and biological studies of some lanthanide(III chloride complexes with a heterocyclic Schiff base ligand

Directory of Open Access Journals (Sweden)

K. Mohanan

2016-07-01

Full Text Available Condensation of 2-hydroxy-1-naphthaldehyde with 2-amino-3-carboxyethyl-4,5-dimethylthiophene in 1:1 molar ratio, yielded a potentially tridentate Schiff base viz. 2-[N-(2′-hydroxy-1-naphthylideneamino]-3-carboxyethyl-4,5-dimethylthiophene (HNAT. This ligand formed complexes with lanthanum(III, cerium(III, praseodymium(III, neodymium(III, samarium(III, europium(III and gadolinium(III chloride under well defined conditions. These complexes were characterized through elemental analysis, molar conductance, magnetic moment measurements, IR, UV–Vis, FAB mass and 1H NMR spectral studies. Analytical data showed that all the metal complexes exhibited 1:1 metal–ligand ratio. Molar conductance values adequately confirmed the non-electrolytic nature of the metal complexes. The proton NMR spectral observations supplement the IR spectral assignments. The spectral data revealed that the ligand acted as neutral tridentate, coordinating to the metal ion through azomethine nitrogen, ester carbonyl and naphtholate oxygen without deprotonation. The ligand and its lanthanum(III chloride complex were subjected to XRD studies. The lanthanum(III chloride complex has undergone a facile transesterification reaction. The solid state d.c. electrical conductivity of some selected complexes were measured as a function of temperature, indicating the semiconducting nature of the metal complexes. The antimicrobial activities were examined by disk diffusion method against some pathogenic bacterial and fungal species.

Thermodynamic study on the complexation of Trivalent actinide and lanthanide cation by N-donor ligands in homogeneous conditions; Etude thermodynamique de la complexation des ions actinide (III) et lanthanide (III) par des ligands polyazotes en milieu homogene

Energy Technology Data Exchange (ETDEWEB)

Miguirditchian, M

2004-07-01

Polydentate N-donor ligands, alone or combined with a synergic acid, may selectively extract minor actinides(III) from lanthanide(III) ions, allowing to develop separation processes of long-live radioelements. The aim of the researches carried out during this thesis was to better understand the chemical mechanisms of the complexation of f-elements by Adptz, a tridentate N-donor ligand, in homogeneous conditions. A thermodynamic approach was retained in order to estimate, from an energetic point of view, the influence of the different contributions to the reaction, and to acquire a complete set of thermodynamic data on this reaction. First, the influence of the nature of the cation on the thermodynamics was considered. The stability constants of the 1/1 complexes were systematically determined by UV-visible spectrophotometry for every lanthanide ion (except promethium) and for yttrium in a mixed solvent methanol/water in volume proportions 75/25%. The thermodynamic parameters ({delta}H{sup 0} {delta}{sup S}) of complexation were estimated by the van't Hoff method and by micro-calorimetry. The trends of the variations across the lanthanide series are compared with similar studies. The same methods were applied to the study of three actinide(III) cations: plutonium, americium and curium. The comparison of these values with those obtained for the lanthanides highlights the increase of stability of these complexes by a factor of 20 in favor of the actinide cations. This gap is explained by a more exothermic reaction and is associated, in the data interpretation, to a higher covalency of the actinide(III)-nitrogen bond. Then, the influence of the change of solvent composition on the thermodynamic of complexation was studied. The thermodynamic parameters of the complexation of europium(III) by Adptz were determined for several fractions of methanol. The stability of the complex formed increases with the percentage of methanol in the mixed solvent, owing to an

Lanthanide complexes with pivaloylacetone

International Nuclear Information System (INIS)

Eliseeva, S.V.; Chugarov, N.V.; Kuz'mina, N.P.; Martynenko, L.I.; Nichiporuk, R.V.; Ivanov, S.A.

2003-01-01

Complexes Ln(pa) 3 ·2H 2 O (Ln=La, Gd, Lu, Hpa - pivaloylacetone) are synthesized and investigated by the methods of element, IR spectroscopic and thermal analyses. Behaviour of the complexes during heating in vacuum is compared with such one for acetylacetonates and dipivaloylmethanates. Structure of the complexes in solution is studied by 1 H NMR and MALDI-MS [ru

Annual reports in inorganic and general syntheses 1974

CERN Document Server

Niedenzu, Kurt

1975-01-01

Annual Reports in Inorganic and General Syntheses-1974 presents an organized annual summary of synthetic developments in inorganic chemistry and its related areas. The book discusses the chemistry of simple and complex metal hydrides of main groups I, II, and III, boron, aluminium, gallium, indium, thallium, silicon, germanium, tin, lead, phosphorus, arsenic, antimony, bismuth, chalcogens, halogens, and pseudohalogens. The text also describes the chemistry of scandium, yttrium, lanthanides, actinides, titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, ma

Theoretical study of the electronic structure of f-element complexes by quantum chemical methods; Analyse de la structure electronique des complexes contenant des elements F par des methodes de la chimie quantique

Energy Technology Data Exchange (ETDEWEB)

Vetere, V

2002-09-15

This thesis is related to comparative studies of the chemical properties of molecular complexes containing lanthanide or actinide trivalent cations, in the context of the nuclear waste disposal. More precisely, our aim was a quantum chemical analysis of the metal-ligand bonding in such species. Various theoretical approaches were compared, for the inclusion of correlation (density functional theory, multiconfigurational methods) and of relativistic effects (relativistic scalar and 2-component Hamiltonians, relativistic pseudopotentials). The performance of these methods were checked by comparing computed structural properties to published experimental data, on small model systems: lanthanide and actinide tri-halides and on X{sub 3}M-L species (X=F, Cl; M=La, Nd, U; L = NH{sub 3}, acetonitrile, CO). We have thus shown the good performance of density functionals combined with a quasi-relativistic method, as well as of gradient-corrected functionals associated with relativistic pseudopotentials. In contrast, functionals including some part of exact exchange are less reliable to reproduce experimental trends, and we have given a possible explanation for this result . Then, a detailed analysis of the bonding has allowed us to interpret the discrepancies observed in the structural properties of uranium and lanthanides complexes, based on a covalent contribution to the bonding, in the case of uranium(III), which does not exist in the lanthanide(III) homologues. Finally, we have examined more sizeable systems, closer to experimental species, to analyse the influence of the coordination number, of the counter-ions and of the oxidation state of uranium, on the metal-ligand bonding. (author)

spectral characterization and dna binding properties of lanthanide(iii)

African Journals Online (AJOL)

nitrogen, azomethine-nitrogen and amido-oxygen donor atoms. .... (singlet 3 H), are respectively assigned to pyridine, isonicotine, -NH and methyl ... In the electronic spectra of complexes a broad peak is observed in the high energy region at.

Theoretical study of the electronic structure of f-element complexes by quantum chemical methods

International Nuclear Information System (INIS)

Vetere, V.

2002-09-01

This thesis is related to comparative studies of the chemical properties of molecular complexes containing lanthanide or actinide trivalent cations, in the context of the nuclear waste disposal. More precisely, our aim was a quantum chemical analysis of the metal-ligand bonding in such species. Various theoretical approaches were compared, for the inclusion of correlation (density functional theory, multiconfigurational methods) and of relativistic effects (relativistic scalar and 2-component Hamiltonians, relativistic pseudopotentials). The performance of these methods were checked by comparing computed structural properties to published experimental data, on small model systems: lanthanide and actinide tri-halides and on X 3 M-L species (X=F, Cl; M=La, Nd, U; L = NH 3 , acetonitrile, CO). We have thus shown the good performance of density functionals combined with a quasi-relativistic method, as well as of gradient-corrected functionals associated with relativistic pseudopotentials. In contrast, functionals including some part of exact exchange are less reliable to reproduce experimental trends, and we have given a possible explanation for this result . Then, a detailed analysis of the bonding has allowed us to interpret the discrepancies observed in the structural properties of uranium and lanthanides complexes, based on a covalent contribution to the bonding, in the case of uranium(III), which does not exist in the lanthanide(III) homologues. Finally, we have examined more sizeable systems, closer to experimental species, to analyse the influence of the coordination number, of the counter-ions and of the oxidation state of uranium, on the metal-ligand bonding. (author)

Enhanced antibacterial activity of zinc oxide nanoparticles synthesized using Petroselinum crispum extracts

Energy Technology Data Exchange (ETDEWEB)

Stan, Manuela, E-mail: manuela.stan@itim-cj.ro; Popa, Adriana; Toloman, Dana; Silipas, Teofil-Danut [National Institute for Research and Development of Isotopic and Molecular Technologies, 67-103 Donat, 400293 Cluj-Napoca (Romania); Vodnar, Dan Cristian [University of Agricultural Sciences and Veterinary Medicine, Department of Food Science and Technology, 3-5 Manastur Street, 400372 Cluj-Napoca (Romania); Katona, Gabriel [Babes-Bolyai University, Faculty of Chemistry and Chemical Engineering, 11 Arany Janos Street, 400028 Cluj-Napoca (Romania)

2015-12-23

The present contribution reports the synthesis of zinc oxide nanoparticles (ZnO NPs) using aqueous leaf and root extracts of Petroselinum crispum (parsley) and characterization of as-prepared samples. ZnO NPs are subjected to X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron paramagnetic resonance (EPR) studies. The XRD studies reveal a hexagonal wurtzite structure without supplementary diffraction lines for all ZnO samples. TEM analysis shows that the particle size is influenced by the type of plant extract. The EPR spectra indicate the presence of Mn{sup 2+} ions in ZnO sample synthesized using P. crispum leaf extract, while zinc vacancy complexes and oxygen vacancies are evidenced in all analyzed samples. ZnO NPs synthesized using P. crispum extracts exhibit increased (2-16 times) antibacterial activity as compared to chemically synthesized ZnO NPs.

Enhanced antibacterial activity of zinc oxide nanoparticles synthesized using Petroselinum crispum extracts

International Nuclear Information System (INIS)

Stan, Manuela; Popa, Adriana; Toloman, Dana; Silipas, Teofil-Danut; Vodnar, Dan Cristian; Katona, Gabriel

2015-01-01

The present contribution reports the synthesis of zinc oxide nanoparticles (ZnO NPs) using aqueous leaf and root extracts of Petroselinum crispum (parsley) and characterization of as-prepared samples. ZnO NPs are subjected to X-ray diffraction (XRD), transmission electron microscopy (TEM) and electron paramagnetic resonance (EPR) studies. The XRD studies reveal a hexagonal wurtzite structure without supplementary diffraction lines for all ZnO samples. TEM analysis shows that the particle size is influenced by the type of plant extract. The EPR spectra indicate the presence of Mn 2+ ions in ZnO sample synthesized using P. crispum leaf extract, while zinc vacancy complexes and oxygen vacancies are evidenced in all analyzed samples. ZnO NPs synthesized using P. crispum extracts exhibit increased (2-16 times) antibacterial activity as compared to chemically synthesized ZnO NPs

Platinum Group Thiophenoxyimine Complexes: Syntheses,Crystallographic and Computational Studies of Structural Properties

Energy Technology Data Exchange (ETDEWEB)

Krinsky, Jamin L.; Arnold, John; Bergman, Robert G.

2006-10-03

Monomeric thiosalicylaldiminate complexes of rhodium(I) and iridium(I) were prepared by ligand transfer from the homoleptic zinc(II) species. In the presence of strongly donating ligands, the iridium complexes undergo insertion of the metal into the imine carbon-hydrogen bond. Thiophenoxyketimines were prepared by non-templated reaction of o-mercaptoacetophenone with anilines, and were complexed with rhodium(I), iridium(I), nickel(II) and platinum(II). X-ray crystallographic studies showed that while the thiosalicylaldiminate complexes display planar ligand conformations, those of the thiophenoxyketiminates are strongly distorted. Results of a computational study were consistent with a steric-strain interpretation of the difference in preferred ligand geometries.

Syntheses and characterization of two new zinc phosphites with 1D chains decorated by Zn-centered complexes

Science.gov (United States)

Zhong, You-Ju; Chen, Yong-Mei; Sun, Yan-Qiong; Yang, Guo-Yu

2005-09-01

Two inorganic-organic hybrid solids, Zn 2(phen)(HPO 3) 2 ( 1) and Zn(phen)(HPO 3) ( 2), have been synthesized under solvothermal conditions in the presence of 1,10-phenanthroline (phen) ligands. Their structures were determined by single-crystal X-ray diffraction and further characterized by FTIR, elemental analysis, powder X-ray diffraction, thermogravimetric analysis and fluorescent spectra. Compound 1 crystallizes in the triclnic system, space group P-1, a=8.1813(3) Å, b=8.5535(3) Å, c=12.3031(5) Å, α=75.609(1)°, β=79.145(2)°, γ=67.157(2)°, V=764.46(5) Å3, Z=2. Compound 2 is monoclinic, C2/c, a=16.1044(7) Å, b=18.9447(6) Å, c=8.1713(6) Å, β=94.175(4)°, V=2486.4(2) Å3, Z=8. Both structures consist of 1D chains constructed from strictly alternating ZnO 4 and HPO 3 polyhedra through sharing vertices. The chains are further decorated by Zn-centered complex architectures, [Zn(phen)] 2+ for 1 and [Zn(phen) 2] 2+ for 2. The 2D and 3D supramolecular arrays for 1 and 2 are stably stacked via strong π- π interactions of the phen groups, respectively.

Syntheses and characterization of two new zinc phosphites with 1D chains decorated by Zn-centered complexes

International Nuclear Information System (INIS)

Zhong Youju; Chen Yongmei; Sun Yanqiong; Yang Guoyu

2005-01-01

Two inorganic-organic hybrid solids, Zn 2 (phen)(HPO 3 ) 2 (1) and Zn(phen)(HPO 3 ) (2), have been synthesized under solvothermal conditions in the presence of 1,10-phenanthroline (phen) ligands. Their structures were determined by single-crystal X-ray diffraction and further characterized by FTIR, elemental analysis, powder X-ray diffraction, thermogravimetric analysis and fluorescent spectra. Compound 1 crystallizes in the triclnic system, space group P-1, a=8.1813(3)A, b=8.5535(3)A, c=12.3031(5)A, α=75.609(1) o , β=79.145(2) o , γ=67.157(2) o , V=764.46(5)A 3 , Z=2. Compound 2 is monoclinic, C2/c, a=16.1044(7)A, b=18.9447(6)A, c=8.1713(6)A, β=94.175(4) o , V=2486.4(2)A 3 , Z=8. Both structures consist of 1D chains constructed from strictly alternating ZnO 4 and HPO 3 polyhedra through sharing vertices. The chains are further decorated by Zn-centered complex architectures, [Zn(phen)] 2+ for 1 and [Zn(phen) 2 ] 2+ for 2. The 2D and 3D supramolecular arrays for 1 and 2 are stably stacked via strong π-π interactions of the phen groups, respectively

Bias Voltage-Dependent Impedance Spectroscopy Analysis of Hydrothermally Synthesized ZnS Nanoparticles

Science.gov (United States)

Dey, Arka; Dhar, Joydeep; Sil, Sayantan; Jana, Rajkumar; Ray, Partha Pratim

2018-04-01

In this report, bias voltage-dependent dielectric and electron transport properties of ZnS nanoparticles were discussed. ZnS nanoparticles were synthesized by introducing a modified hydrothermal process. The powder XRD pattern indicates the phase purity, and field emission scanning electron microscope image demonstrates the morphology of the synthesized sample. The optical band gap energy (E g = 4.2 eV) from UV measurement explores semiconductor behavior of the synthesized material. The electrical properties were performed at room temperature using complex impedance spectroscopy (CIS) technique as a function of frequency (40 Hz-10 MHz) under different forward dc bias voltages (0-1 V). The CIS analysis demonstrates the contribution of bulk resistance in conduction mechanism and its dependency on forward dc bias voltages. The imaginary part of the impedance versus frequency curve exhibits the existence of relaxation peak which shifts with increasing dc forward bias voltages. The dc bias voltage-dependent ac and dc conductivity of the synthesized ZnS was studied on thin film structure. A possible hopping mechanism for electrical transport processes in the system was investigated. Finally, it is worth to mention that this analysis of bias voltage-dependent dielectric and transport properties of as-synthesized ZnS showed excellent properties for emerging energy applications.

A general digital computer procedure for synthesizing linear automatic control systems

International Nuclear Information System (INIS)

Cummins, J.D.

1961-10-01

The fundamental concepts required for synthesizing a linear automatic control system are considered. A generalized procedure for synthesizing automatic control systems is demonstrated. This procedure has been programmed for the Ferranti Mercury and the IBM 7090 computers. Details of the programmes are given. The procedure uses the linearized set of equations which describe the plant to be controlled as the starting point. Subsequent computations determine the transfer functions between any desired variables. The programmes also compute the root and phase loci for any linear (and some non-linear) configurations in the complex plane, the open loop and closed loop frequency responses of a system, the residues of a function of the complex variable 's' and the time response corresponding to these residues. With these general programmes available the design of 'one point' automatic control systems becomes a routine scientific procedure. Also dynamic assessments of plant may be carried out. Certain classes of multipoint automatic control problems may also be solved with these procedures. Autonomous systems, invariant systems and orthogonal systems may also be studied. (author)

Synthesis and complexation properties towards uranyl cation of carboxylic acid derivatives of p-tert-butyl-calix[6]arene; Synthese et proprietes complexantes vis-a-vis de l'ion uranyle de derives carboxyliques du p-tert-butyl-calix[6]arene

Energy Technology Data Exchange (ETDEWEB)

Souane, R

2005-03-15

In the fuel reprocessing plants radioactive metals, and more particularly, uranium in UO{sub 2}{sup 2+} form in the various installations, have many varied physico-chemical forms and there is a risk of exposure and internal contamination in the nuclear industry. It is necessary to exert a medical control to ensure the protection of the health of the workers. This medical control is done by dosing uranyl cation in the urine of the exposed people. This work forms part of this context. Indeed, we prepared a ligand able to complex the ion uranyl and which is also to be grafted on a solid support. In the family of calixarenes, the calix[6]arenes functionalized by three or four carboxylic functions were selected like chelating molecules of the ion uranyl. The properties of complexation of these calixarenes were studied by potentiometry in methanol, under these conditions balances of protonation and complexation were determined and the constant partners were obtained using the Hyperquad program. We synthesized tri-carboxylic calix[6]arenes comprising of the groupings nitro (NO{sub 2}) in para position of phenol in order to see the influence of a substitution in para position on the complexation. We also synthesized calix[6]arenes tetra-carboxylic in order to show the role of an additional carboxylic acid grouping. The potentiometric study determined thermodynamic parameters of protonation and complexation of carboxylic calix[6]arenes. The results of the complexation highlighted which complex UO{sub 2}L corresponding to the ligand para-tert-butyl-calix[6]arene tetra-acid is more stable than that corresponding to the ligand mono-nitro calix[6]arene tri-acid ({delta}log{beta}110 = 4.3), and than the effect of the groupings nitro in para position has low influence on the complexation of UO{sub 2}{sup 2+}. This makes it possible to consider as possible the grafting of the calix[6]arenes which one knows the behaviour of trapping. To this end we synthesized the ligand 23

Mew organometallic complexes of technetium in different oxidation states

International Nuclear Information System (INIS)

Joachim, J.E.

1993-09-01

New organometallic compounds of Tc(I), Tc(III) and Tc(VII) were synthesized and their properties examined. These compounds were correlated with their homologous compounds of manganese and rhenium, which were also synthesized by the same route. The molecular and crystal structures of most technetium complexes and of the homologous complexes of manganese and rhenium were determined by single crystal X-ray diffraction. (orig.) [de

Thermodynamics of complexation of lanthanides and some of transition metal ions by 5,5-dimethyl-cyclohexane-2-(2-hydroxyphenyl)-hydrazono-1,3-dione (DCPHD) and its derivatives

International Nuclear Information System (INIS)

Ramadan, A.A.T.; Abdel-Moez, M.S.; El-Shetary, B.A.; Seleim, H.S.

1993-01-01

Equilibrium between DCPHD, DC-4-Cl-PHD, and DC-4-Me-PHD and protons, transition, and lanthanide ions have been investigated at 30 o C by means of potentiometric titration in 75%(v/v) methanol-water mixture containing 0.10M KNO 3 as a constant ionic medium. Thermodynamic parameters(ΔG,ΔH and ΔS) referring to the formation of species HL - ,L -- ,ML +n-2 and ML 2 +n-4 (L -- denotes the ligand anion) have been determined in solutions. The solvent effects on the thermodynamic parameters of the complex formation are discussed in terms of differences in the donor ability of methanol and water solvents. The plots of thermodynamic parameters versus ionic potential (Z 2 /r) of the lanthanide elements is not linear as expected from ionic theory. The obtained curve can be resolved in an initial group (the lighter lanthanides), an intermediate group (Sm-Dy), and a final group (the heavier ones, Tb-Lu). This behavior was explained in terms of differences in the dehydration of lighter lanthanide(III) from that of heavier ones

Implementation of Different Variants of Table-Based Frequency Synthesizers with Quadrature Output in VHDL

Directory of Open Access Journals (Sweden)

Daniel Kekrt

2012-01-01

Full Text Available This article describes the modelling and implementation of two different variants of direct frequency synthesizer, and evaluation of the performance of the finished design, in terms of memory and speed efficiency. The frequency synthesizer requirement comes from our complex radio transmission system design. The research activity has been focused on finding an optimal balance between simplicity, speed and memory consumption. The modelling was done in MATLAB environment in floating-point and fixed-point arithmetic, and the actual design was implemented and synthesized using the Xilinx ISE suite. The output has been connected to our customized radio front-end built on the Texas Instruments TRF2443 chip. The front-end output signal has been captured and compared with simulation results.

Analysis of Periodic Errors for Synthesized-Reference-Wave Holography

Directory of Open Access Journals (Sweden)

V. Schejbal

2009-12-01

Full Text Available Synthesized-reference-wave holographic techniques offer relatively simple and cost-effective measurement of antenna radiation characteristics and reconstruction of complex aperture fields using near-field intensity-pattern measurement. These methods allow utilization of advantages of methods for probe compensations for amplitude and phasing near-field measurements for the planar and cylindrical scanning including accuracy analyses. The paper analyzes periodic errors, which can be created during scanning, using both theoretical results and numerical simulations.

Copper-based metal coordination complexes with Voriconazole ligand: Syntheses, structures and antimicrobial properties

Science.gov (United States)

Zhao, Yan-Ming; Tang, Gui-Mei; Wang, Yong-Tao; Cui, Yue-Zhi; Ng, Seik Weng

2018-03-01

Three new chiral metal coordination complexes, namely, [Cu(FZ)2(CH3COO)2(H2O)]·2H2O (1), [Cu(FZ)2(NO3)2] (2), and [Cu2(FZ)2 (H2O)8](SO4)2·4H2O (3) [FZ = (2R,3S)-2-(2,4-difluorophenyl)-3-(5-fluoro-4-pyrimidiny)-1-(1H-1,2,4-triazol-1-yl)-2-butanol) (Voriconazole)] have been obtained by the reaction of Cu(II) salts and the free ligand FZ at room temperature. Complexes 1-3 were structurally characterized by X-ray single-crystal diffraction, IR, UV-vis, powder X-ray diffraction (PXRD), and thermogravimetric analysis (TGA). Complex 1 crystallizes in the chiral space group C2, which exhibits a mono-nuclear structure. Both complexes 2 and 3 display a one-dimensional (1D) tape structure, which crystallize in chiral space group P21212 and P212121, respectively. Among these complexes, there exist a variety of hydrogen bonds and stacking interactions, through which a three-dimensional supramolecular architecture will be generated. Compared with the standard (Voriconazole), these Cu-based complexes show the more potent inhibiting efficiency against the species of Candida and Aspergillus. Moreover, among these complexes, complex 1 shows the most excellent efficiency.

Characterization of gadolinia-doped ceria with manganese addition synthesized by the cation complexation technique; Caracterizacao de ceria-gadolinia e ceria-gadolinia-manganes sintetizados pelo metodo de complexacao de cations

Energy Technology Data Exchange (ETDEWEB)

Yang, J.D.; Muccillo, R.; Muccillo, E.N.S., E-mail: enavarro@usp.b [Instituto de Pesquisas Energeticas e Nucleares (CCTM/IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Ciencia e Tecnologia de Materiais; Rocha, R.A. [Universidade Federal do ABC (CEMCSA/UFABC), Santo Andre, SP (Brazil). Centro de Engenharia, Modelagem e Ciencias Sociais Aplicadas

2010-07-01

Ceria-based compounds may be used for several technological applications like catalysts, grinding media and materials for electrolyte and electrodes in solid oxide fuel cells. For most of these applications fine powders are required. In this work, nanostructured ceria powders containing 20 mol % gadolinia with and without manganese addition were synthesized by the cation complexation technique. The prepared powders were calcined at 600 deg C for thermal decomposition of the metal citrate precursors. Results of X-ray diffraction, scanning electron microscopy and specific surface area evidenced the role of manganese on physical characteristics of the nanostructured materials. The cation complexation technique revealed to be a promising method for obtaining nanostructured powders with high yield and suitable physical properties for several technological applications. (author)

Evaluation of immunoglobulin G synthesizing plasma cells in periapical granuloma and cyst.

OpenAIRE

Grover N; Rao N; Kotian M

2001-01-01

Immunoglobulin synthesizing plasma cells for IgG were quantitated in 20 periapical granulomas and 20 periapical cysts, using unlabelled antibody peroxidase-antiperoxidase complex method. Result showed that immunoglobulin G producing plasma cells were predominant in periapical cyst as compared with periapical granuloma. A statistical significant relation was observed between these two lesions.

Lanthanide complexes of macrocyclic polyoxovanadates by VO4 units: synthesis, characterization, and structure elucidation by X-ray crystallography and EXAFS spectroscopy.

Science.gov (United States)

Nishio, Masaki; Inami, Shinnosuke; Katayama, Misaki; Ozutsumi, Kazuhiko; Hayashi, Yoshihito

2012-01-16

Reactions of a tetravanadate anion, [V(4)O(12)](4-), with a series of lanthanide(III) salts yield three types of lanthanide complexes of macrocyclic polyoxovanadates: (Et(4)N)(6)[Ln(III)V(9)O(27)] [Ln = Nd (1), Sm (2), Eu (3), Gd (4), Tb (5), Dy (6)], (Et(4)N)(5)[(H(2)O)Ho(III)(V(4)O(12))(2)] (7), and (Et(4)N)(7)[Ln(III)V(10)O(30)] [Ln = Er (8), Tm (9), Yb (10), Lu (11)]. Lanthanide complexes 1-11 are isolated and characterized by IR, elemental analysis, single-crystal X-ray diffraction, and extended X-ray absorption fine structure spectroscopy (EXAFS). Lanthanide complexes 1-6 are composed of a square-antiprism eight-coordinated Ln(III) center with a macrocyclic polyoxovanadate that is constructed from nine VO(4) tetrahedra through vertex sharing. The structure of 7 is composed of a seven-coordinated Ho(III) center, which exhibits a capped trigonal-prism coordination environment by the sandwiching of two cyclic tetravanadates with a capping H(2)O ligand. Lanthanide complexes 8-11 have a six-coordinated Ln(III) center with a 10-membered vanadate ligand. The structural trend to adopt a larger coordination number for a larger lanthanide ion among the three types of structures is accompanied by a change in the vanadate ring sizes. These lanthanide complexes are examined by EXAFS spectroscopies on lanthanide L(III) absorption edges, and the EXAFS oscillations of each of the samples in the solid state and in acetonitrile are identical. The Ln-O and Ln···V bond lengths obtained from fits of the EXAFS data are consistent with the data from the single-crystal X-ray studies, reflecting retention of the structures in acetonitrile.

Design principles and theory of paramagnetic fluorine-labelled lanthanide complexes as probes for (19)F magnetic resonance: a proof-of-concept study.

Science.gov (United States)

Chalmers, Kirsten H; De Luca, Elena; Hogg, Naomi H M; Kenwright, Alan M; Kuprov, Ilya; Parker, David; Botta, Mauro; Wilson, J Ian; Blamire, Andrew M

2010-01-04

The synthesis and spectroscopic properties of a series of CF(3)-labelled lanthanide(III) complexes (Ln=Gd, Tb, Dy, Ho, Er, Tm) with amide-substituted ligands based on 1,4,7,10-tetraazacyclododecane are described. The theoretical contributions of the (19)F magnetic relaxation processes in these systems are critically assessed and selected volumetric plots are presented. These plots allow an accurate estimation of the increase in the rates of longitudinal and transverse relaxation as a function of the distance between the Ln(III) ion and the fluorine nucleus, the applied magnetic field, and the re-rotational correlation time of the complex, for a given Ln(III) ion. Selected complexes exhibit pH-dependent chemical shift behaviour, and a pK(a) of 7.0 was determined in one example based on the holmium complex of an ortho-cyano DO3A-monoamide ligand, which allowed the pH to be assessed by measuring the difference in chemical shift (varying by over 14 ppm) between two (19)F resonances. Relaxation analyses of variable-temperature and variable-field (19)F, (17)O and (1)H NMR spectroscopy experiments are reported, aided by identification of salient low-energy conformers by using density functional theory. The study of fluorine relaxation rates, over a field range of 4.7 to 16.5 T allowed precise computation of the distance between the Ln(III) ion and the CF(3) reporter group by using global fitting methods. The sensitivity benefits of using such paramagnetic fluorinated probes in (19)F NMR spectroscopic studies are quantified in preliminary spectroscopic and imaging experiments with respect to a diamagnetic yttrium(III) analogue.

Complexing Agents on Carbon Content and Lithium Storage Capacity of LiFePO4/C Cathode Synthesized via Sol-Gel Approach

Directory of Open Access Journals (Sweden)

C. Guan

2016-01-01

Full Text Available Olivine-structured LiFePO4 faces its intrinsic challenges in terms of poor electrical conductivity and lithium-ion diffusion capability for application to lithium-ion batteries. Cost-effective sol-gel approach is advantageous to in situ synthesize carbon-coated LiFePO4 (LiFePO4/C which can not only improve electronic conductivity but also constrain particle size to nanometer scale. In this study, the key parameter is focused on the choice and amount of chelating agents in this synthesis route. It was found that stability of complexing compounds has significant impacts on the carbon contents and electrochemical properties of the products. At the favorable choice of precursors, composition, and synthesis conditions, nanocrystalline LiFePO4/C materials with appropriate amount of carbon coating were successfully obtained. A reversible capacity of 162 mAh/g was achieved at 0.2C rate, in addition to good discharge rate capability.

Biological activities of some Fluoroquinolones-metal complexes

African Journals Online (AJOL)

McRoy

DNA cleavage studies of some synthesized metal complexes of fluoroquinolone ... Although the FQs are generally characterized by a broad antimicrobial spectrum ..... six Coordinate 3rd metal complexes with N- (5 –Phenyl-3,4- thiadiazol-2-yl).

Fabrication of copper-selective PVC membrane electrode based on newly synthesized copper complex of Schiff base as carrier

Directory of Open Access Journals (Sweden)

Sulekh Chandra

2016-09-01

Full Text Available The newly synthesized copper(II complex of Schiff base p-hydroxyacetophenone semicarbazone was explored as neutral ionophore for the fabrication of poly(vinylchloride (PVC based membrane electrode selective to Cu(II ions. The electrode shows a Nernstian slope of 29.8 ± 0.3 mV/decade with improved linear range of 1.8 × 10−7 to 1.0 × 10−1 M, comparatively lower detection limit 5.7 × 10−8 M between pH range of 2.0–8.0, giving a relatively fast response within 5s and can be used for at least 16 weeks without any divergence in potential. The selectivity coefficient was calculated using the fixed interference method (FIM. The electrode can also be used in partially non-aqueous media having up to 25% (v/v methanol, ethanol or acetone content with no significant change in the value of slope or working concentration range. It was successfully applied for the direct determination of copper content in water and tea samples with satisfactory results. The electrode has been used in the potentiometric titration of Cu2+ with EDTA.

Zirconium (IV) complexes with some polymethylenediimines | Na ...

African Journals Online (AJOL)

The syntheses of zirconium (IV) complexes have been carried out by the reaction of oxozirconium (IV) chloride with the appropriate diimines (Schiff bases). The complexes were isolated as yellow solids which are stable to heat. The complexes were found to be insoluble in most solvents. The infrared spectra, elemental ...

Integrated digital superconducting logic circuits for the quantum synthesizer. Report

International Nuclear Information System (INIS)

Buchholz, F.I.; Kohlmann, J.; Khabipov, M.; Brandt, C.M.; Hagedorn, D.; Balashov, D.; Maibaum, F.; Tolkacheva, E.; Niemeyer, J.

2006-11-01

This report presents the results, which were reached in the framework of the BMBF cooperative plan ''Quantum Synthesizer'' in the partial plan ''Integrated Digital Superconducting Logic Circuits''. As essential goal of the plan a novel instrument on the base of quantum-coherent superconducting circuits should be developed. which allows to generate praxis-relevant wave forms with quantum accuracy, the quantum synthesizer. The main topics of development of the reported partial plan lied at the one hand in the development of integrated, digital, superconducting circuit in rapid-single-flux (RSFQ) quantum logics for the pattern generator of the quantum synthesizer, at the other hand in the further development of the fabrication technology for the aiming of high circuit complexity. In order to fulfil these requirements at the PTB a new design system was implemented, based on the software of Cadence. Together with the required RSFQ extensions for the design of digital superconducting circuits was a platform generated, on which the reachable circuit complexity is exclusively limited by the technology parameters of the available fabrication technology: Physical simulations are with PSCAN up to a complexity of more than 1000 circuit elements possible; furthermore VHDL allows the verification of arbitrarily large circuit architectures. In accordance for this the production line at the PTB was brought to a level, which allows in Nb/Al-Al x O y /Nb SIS technology implementation the fabrication of highly integrable RSFQ circuit architectures. The developed and fabricated basic circuits of the pattern generator have proved correct functionality and reliability in the measuring operation. Thereby for the circular RSFQ shift registers a key role as local memories in the construction of the pattern generator is devolved upon. The registers were realized with the aimed bit lengths up to 128 bit and with reachable signal-processing speeds of above 10 GHz. At the interface RSFQ

Expedient Syntheses of Neutral and Cationic Au(I)–NHC Complexes

KAUST Repository

Veenboer, Richard M. P.

2017-09-08

The synthesis and isolation of gold(I) precatalysts often requires the generation of several isolable intermediates as well as numerous purification steps. New protocols for the expedient synthesis of neutral [Au(OH)(NHC)] and [Au(CH2COCH3)(NHC)] species from [AuCl(NHC)] or [AuCl(DMS)] precursors bearing a variety of N-heterocyclic carbene (NHC) ligands are presented. These methods can be employed in a telescoping manner for the synthesis of catalytically relevant [Au(NTf2)(NHC)] and [Au(NHC)(NCCH3)][BF4] complexes. These attractive methods are straightforward and practical leading to various complexes in high isolated yields and purity.

Expedient Syntheses of Neutral and Cationic Au(I)–NHC Complexes

KAUST Repository

Veenboer, Richard M. P.; Gasperini, Danila; Nahra, Fady; Cordes, David B.; Slawin, Alexandra M. Z.; Cazin, Catherine S. J.; Nolan, Steven P.

2017-01-01

The synthesis and isolation of gold(I) precatalysts often requires the generation of several isolable intermediates as well as numerous purification steps. New protocols for the expedient synthesis of neutral [Au(OH)(NHC)] and [Au(CH2COCH3)(NHC)] species from [AuCl(NHC)] or [AuCl(DMS)] precursors bearing a variety of N-heterocyclic carbene (NHC) ligands are presented. These methods can be employed in a telescoping manner for the synthesis of catalytically relevant [Au(NTf2)(NHC)] and [Au(NHC)(NCCH3)][BF4] complexes. These attractive methods are straightforward and practical leading to various complexes in high isolated yields and purity.

Encapsulation of ferro- and ferricyanide complexes inside ZSM-5 zeolite synthesized from rice straw: Implications for synthesis of Prussian blue pigment

International Nuclear Information System (INIS)

Ali, Ibraheem O.; Salama, Tarek M.; Thabet, Mohamed S.; El-Nasser, Karam S.; Hassan, Ali M.

2013-01-01

Encapsulation of [Fe(CN) 6 ] 4− and [Fe(CN) 6 ] 3− complexes in the intracrystalline pores of ZSM-5 zeolite, Fe II L/Z and Fe III L/Z respectively, by the zeolite synthesis method was reported. The modified zeolites were characterized by powder XRD, FT-IR and UV–vis spectroscopy. The nitrogen adsorption isotherms allow for the evaluation of pore structure of the complex-modified zeolites, whereas the thermal analysis (TGA/DTA) measurements provide insight into the decomposition products of the immobilized complexes. The modified zeolites exhibited smaller pore volumes and surface areas as compared with those of unpromoted ZSM-5, suggesting the inclusion of iron cyanides inside the interconnecting channels of ZSM-5. While the ferricyanide complex enhanced the formation of highly crystalline zeolite, the ferrocyanide one resulted in a lesser effect. The electronic spectra of the colloidal species developed when Fe III L/Z brought in contact with an aqueous solution of [Fe(CN) 6 ] 3− exhibit absorptions attributed to CN − → iron charge-transfer. New bands at 294 and 319 nm due to d–d transitions of Fe III tetrahedral monomeric moieties were emitted concurrently under successive adsorption of [Fe(CN) 6 ] aq 3− over Fe III L/Z, along with a broad band at 555 nm assigned to polymeric [Fe II –C–N–Fe III ] of Prussian blue (PB). The FT-IR spectra of Fe III/II L/Z devoted to the adsorption of an aqueous solution of [Fe(CN) 6 ] 3− showed a band at 2092 cm −1 assigned to the C–N stretch in the Fe II –CN–Fe III linkages. The vibrations attributable to Fe–O–Si bonding along with hydrocarbon and nitroprusside appeared only in the spectrum of Fe III L/Z, thus was found to be strong evidence for the mutual interaction between [Fe(CN) 6 ] 3− and the latter sample. - Highlights: • We synthesized ferrous and ferric cyanide complexes inside ZSM-5 zeolite. • The decomposition of the encapsulated complexes occurred at high temperatures. �

A low-jitter RF PLL frequency synthesizer with high-speed mixed-signal down-scaling circuits

International Nuclear Information System (INIS)

Tang Lu; Wang Zhigong; Xue Hong; He Xiaohu; Xu Yong; Sun Ling

2010-01-01

A low-jitter RF phase locked loop (PLL) frequency synthesizer with high-speed mixed-signal down-scaling circuits is proposed. Several techniques are proposed to reduce the design complexity and improve the performance of the mixed-signal down-scaling circuit in the PLL. An improved D-latch is proposed to increase the speed and the driving capability of the DMP in the down-scaling circuit. Through integrating the D-latch with 'OR' logic for dual-modulus operation, the delays associated with both the 'OR' and D-flip-flop (DFF) operations are reduced, and the complexity of the circuit is also decreased. The programmable frequency divider of the down-scaling circuit is realized in a new method based on deep submicron CMOS technology standard cells and a more accurate wire-load model. The charge pump in the PLL is also realized with a novel architecture to improve the current matching characteristic so as to reduce the jitter of the system. The proposed RF PLL frequency synthesizer is realized with a TSMC 0.18-μm CMOS process. The measured phase noise of the PLL frequency synthesizer output at 100 kHz offset from the center frequency is only -101.52 dBc/Hz. The circuit exhibits a low RMS jitter of 3.3 ps. The power consumption of the PLL frequency synthesizer is also as low as 36 mW at a 1.8 V power supply. (semiconductor integrated circuits)

New Transition metal assisted complex borohydrides for hydrogen storage

International Nuclear Information System (INIS)

Sesha Srinivasan; Elias Lee Stefanakos; Yogi Goswami

2006-01-01

High capacity hydrogen storage systems are indeed essential for the on-board vehicular application that leads to the pollution free environment. Apart from the various hydrogen storage systems explored in the past, complex hydrides involving light weight alkali/alkaline metals exhibits promising hydrogenation/ dehydrogenation characteristics. New transition metal assisted complex borohydrides [Zn(BH 4 ) 2 ] have been successfully synthesized by an inexpensive mechano-chemical process. These complex hydrides possesses gravimetric hydrogen storage capacity of ∼8.4 wt.% at around 120 C. We have determined the volumetric hydrogen absorption and desorption of these materials for a number of cycles. Another complex borohydride mixture LiBH 4 /MgH 2 catalyzed with ZnCl 2 has been synthesized and characterized using various analytical techniques. (authors)

Nitrosyl complexes of technetium; Nitrosylkomplexe des Technetiums

Energy Technology Data Exchange (ETDEWEB)

Ackermann, Janine

2016-09-22

The presented thesis describes syntheses and characterization of novel technetium nitrosyl compounds with various ligand systems. The main focus is the synthesis of low-valent technetium nitrosyl complexes with cyclopentadienyl ligands. [German] Gegenstand der vorliegenden Arbeit ist die Synthese und Charakterisierung neuer Technetiumnitrosylverbindungen mit unterschiedlichen Ligandensystemen. Hauptaugenmerk wurde dabei auf die Darstellung niedervalenter Tc(NO)-Verbindungen mit Cyclopentadienyl-Liganden gelegt.

Structural and thermodynamic aspects of aqueous solution of trivalent lanthanides complexation by hydrophobic compounds of tartaric acid, by gluconic acid and related molecules. Outlook for liquid-liquid extraction of these cations

International Nuclear Information System (INIS)

Giroux, Sebastien

1999-01-01

This work deals with the complexation of lanthanide(III) ions by different molecules and with the synthesis of hydrophobic molecules able to extract them of an aqueous solution. Its aim is to describe the systems obtained by the determination of the formation constants of the species and by the description of their structure. The aim of this work is also to obtain a selective complexation of lanthanides(III) towards actinides(III), because this aim presents a great interest in the reprocessing of radioactive wastes. The complexation studies have been followed by potentiometry, NMR, UV-visible spectroscopy and circular dichroism. The first mixtures studied are the couples: lanthanide(III)-gluconic acid (LH). The complexes system they formed has been described and the structures have been specified; a strong complexation has been revealed. The MLH -2 specie induces a selectivity between the lanthanides(III) equivalent to those obtained with EDTA and its uncharged character allows to consider the use of gluconic acid as extractant. The use of ligands as glucosaminic acid or glucamine slows the beginning of the complexation until pH= 6-7. The neutral specie MLH -2 is formed too. In order to use the complexing properties of gluconic acid and its selective character towards lanthanides(III), the synthesis of molecules derived containing a long alkyl chain with a hydrophobic character has been carried out for using them as extracting agents. An original method of the preparation of tartramides is presented. This preparation consists of an amidation of one of the carboxylic functions of the tartaric acid by a fatty amine. These molecules, surface-active, complex the lanthanides(III) and extract them in an organic phase using the tri-n-butyl phosphate as co-extractant. (O.M.)

Syntheses of polystyrene supported chelating resin containing the Schiff base derived from salicylaldehyde and triethylene tetramine and its copper(II), nickel(II), cobalt(II), iron(III), zinc(II), cadmium(II), molybdenum(VI), zirconium(IV) and uranium(VI) complexes

International Nuclear Information System (INIS)

Syamal, A.; Singh, M.M.

1998-01-01

A new polymer-anchored chelating ligand has been synthesized by the reaction of chloromethylated polystyrene (containing 0.94 mmol of Cl per gram of resin and 1% cross-linked with divinylbenzene) and the Schiff base derived from salicylaldehyde and triethylenetetramine. A new series of polystyrene supported, Cu(II), Ni(II), Co(II), Fe(III), Zn(II), Cd(II), Zr(IV), dioxomolybdenum (VI) and dioxouranium (VI) complexes of the formulae PS-LCu, PS-LNi, PS-LCo, PS-LFeCl.DMF, PS-LZn, PS-LCd, PS-LZr(OH) 2 . DMF, PS L MoO 2 and PS-LUO 2 (where PS-LH 2 = polymer-anchored Schiff base and DMF dimethyl-formamide) have been synthesized and characterised by elemental analysis, infrared, electronic spectra and magnetic susceptibility measurements. The complexes PS-LCu, PS-LNi and PS-LCo have square planar structure, PS-LFeCl.DMF, PS-LMoO 2 and PS-LUO 2 have octahedral structure, PS L Zn and PS-LCd are tetrahedral and PS-LZr(OH) 2 .DMF is pentagonal bipyramidal. The polymer-anchored Cu(II), Co(II) and Fe(III) complexes are paramagnetic while Ni(II), Zn(II), Cd(II), Zr(IV), dioxomolybdenum(VI) and dioxouranium(VI) complexes are diamagnetic. The negative shift of the v (C=N) (azomethine) and the positive shift of v (C--O)(phenolic) are indicative of ONNO donor behaviour of the polymer-anchored Schiff base. (author)

Cobalt (III) complexes as novel matrix metalloproteinase-9 inhibitors

International Nuclear Information System (INIS)

Lee, Jiyoun

2012-01-01

We have synthesized a series of novel MMP-9 inhibitors containing cobalt(III) complexes. The synthesized cobalt(III) complexes are effective as enzyme inhibitors and the attachment of a biphenyl group enhanced the efficiency of enzyme inhibition up to 6-fold. When compared to the reported non-hydroxamate MMP inhibitors, the synthesized complexes showed comparable in vitro potency. The enzyme assay showed that the cobalt(III) complex can disrupt the zinc binding active site of MMP-9 and is proposed to work via a ligand exchange mechanism. Since histidine residues are essential for the catalytic activity of a large percentage of enzymes and zinc finger proteins, these cobalt(III) complexes can serve as a prototype inhibitor towards various zinc containing enzymes and proteins. Matrix metalloproteinases (MMPs) are a family of zinc binding endopeptidases that play crucial roles in various physiological processes and diseases such as embryogenic growth, angiogenesis, arthritis, skin ulceration, liver fibrosis and tumor metastasis. Because of their implications in a wide range of diseases, MMPs are considered as intriguing drug targets. The majority of MMP inhibitors are organic small molecules containing a hydroxamate functionality for the zinc binding group. This hydroxamate group binds to a zinc(II) center in a bidentate fashion and creates a distorted trigonal bipyramidal geometry

Cobalt (III) complexes as novel matrix metalloproteinase-9 inhibitors

Energy Technology Data Exchange (ETDEWEB)

Lee, Jiyoun [Sungshin Women' s Univ., Seoul (Korea, Republic of)

2012-04-15

We have synthesized a series of novel MMP-9 inhibitors containing cobalt(III) complexes. The synthesized cobalt(III) complexes are effective as enzyme inhibitors and the attachment of a biphenyl group enhanced the efficiency of enzyme inhibition up to 6-fold. When compared to the reported non-hydroxamate MMP inhibitors, the synthesized complexes showed comparable in vitro potency. The enzyme assay showed that the cobalt(III) complex can disrupt the zinc binding active site of MMP-9 and is proposed to work via a ligand exchange mechanism. Since histidine residues are essential for the catalytic activity of a large percentage of enzymes and zinc finger proteins, these cobalt(III) complexes can serve as a prototype inhibitor towards various zinc containing enzymes and proteins. Matrix metalloproteinases (MMPs) are a family of zinc binding endopeptidases that play crucial roles in various physiological processes and diseases such as embryogenic growth, angiogenesis, arthritis, skin ulceration, liver fibrosis and tumor metastasis. Because of their implications in a wide range of diseases, MMPs are considered as intriguing drug targets. The majority of MMP inhibitors are organic small molecules containing a hydroxamate functionality for the zinc binding group. This hydroxamate group binds to a zinc(II) center in a bidentate fashion and creates a distorted trigonal bipyramidal geometry.

Preparation of Conductive Organometallic Complexes and Their Pastes or Inks Using the Electron Beam Apparatus

International Nuclear Information System (INIS)

Gu, Ja Min; Lee, Hyosun; Lee, Byung Cheol; Park, Ji Hyun

2011-01-01

We have synthesized the silver and copper complexes using the ligands, amine derivatives Ν-methylhydantoin amine, Ν-triethanol amine, the copper complexes are prepared depending on the equivalents of starting materials, however the silver complexes failed. In case of terephthalic acid, glutaric acid, we have synthesized silver and copper complexes successfully. We have measured conductivity of silver and copper complexes paste and ink themselves by thermal reduction using PULSE UV method. A couple of synthesized copper complex's paste have shown some resistance which is not enough for the conductive materials. Commercially silver pastes composed of silver oxide and silver salt of carboxylic acid, applied to the printed transistor circuits with suitable process, i. e. thermal reduction. This process substituted for electron beam brings a simplification of process, economical, environmental friendly process and a development of in the application of flexible substrate

Chemistry of Iron N -heterocyclic carbene complexes: Syntheses, structures, reactivities, and catalytic applications

KAUST Repository

Riener, Korbinian

2014-05-28

Iron is the most abundant transition metal in Earth\\'s crust. It is relatively inexpensive, not very toxic, and environmentally benign. Undoubtedly, due to the involvement in a multitude of biological processes, which heavily rely on the rich functionalities of iron-containing enzymes, iron is one of the most important elements in nature. Additionally, three-coordinate iron complexes have been reported during the past several years. In this review, the mentioned iron NHC complexes are categorized by their main structure and reactivity attributes. Thus, monocarbene and bis-monocarbene complexes are presented first. This class is subdivided into carbonyl, nitrosyl, and halide compounds followed by a brief section on other, more unconventional iron NHC motifs. Subsequently, donor-substituted complexes bearing bi-, tri-, tetra-, or even pentadentate ligands and further pincer as well as scorpionato motifs are described.

PULSE SYNTHESIZING GENERATOR

Science.gov (United States)

Kerns, Q.A.

1963-08-01

>An electronlc circuit for synthesizing electrical current pulses having very fast rise times includes several sinewave generators tuned to progressively higher harmonic frequencies with signal amplitudes and phases selectable according to the Fourier series of the waveform that is to be synthesized. Phase control is provided by periodically triggering the generators at precisely controlled times. The outputs of the generators are combined in a coaxial transmission line. Any frequency-dependent delays that occur in the transmission line can be readily compensated for so that the desired signal wave shape is obtained at the output of the line. (AEC)

Azido, triazolyl, and alkynyl complexes of gold(I): syntheses, structures, and ligand effects.

Science.gov (United States)

Robilotto, Thomas J; Deligonul, Nihal; Updegraff, James B; Gray, Thomas G

2013-08-19

Gold(I) triazolyl complexes are prepared in [3 + 2] cycloaddition reactions of (tertiary phosphine)gold(I) azides with terminal alkynes. Seven such triazolyl complexes, not previously prepared, are described. Reducible functional groups are accommodated. In addition, two new (N-heterocyclic carbene)gold(I) azides and two new gold(I) alkynyls are described. Eight complexes are crystallographically authenticated; aurophilic interactions appear in one structure only. The packing diagrams of gold(I) triazolyls all show intermolecular hydrogen bonding between N-1 of one molecule and N-3 of a neighbor. This hydrogen bonding permeates the crystal lattice. Density-functional theory calculations of (triphenylphosphine)gold(I) triazolyls and the corresponding alkynyls indicate that the triazolyl is a stronger trans-influencer than is the alkynyl, but the alkynyl is more electron-releasing. These results suggest that trans-influences in two-coordinate gold(I) complexes can be more than a simple matter of ligand donicity.

Synthesis and studies of some magnesium complexes of aromatic hydrazones

International Nuclear Information System (INIS)

Adeniyi, A.A.; Oyedeji, O.O.; Aremu, J.A.; Okedeyi, J.O.; Bourne, S.A.

2006-01-01

Six esters were synthesized from their parent acids, while their corresponding hydrazides were subsequently synthesized from these asters. The hydrazides, on reaction with benzaldehyde, produced their respective hydrazones, namely, benzoic hydrazone (BH), m-nitrobenzoic hydrazone (m-NBH), p-nitrobenzoic hydrazone (p-NBH), 3,5 dinitrobenzoic hydrazone (3,5-dnbh), m-aminobenzoic hydrazone (m-ABH), and p-aminobenzoic hydrazone (p-ABH). These hydrazones, on interaction with magnesium chloride yielded their corresponding magnesium complexes. These complexes were off-white, grey or brownish in colour. These complexes were characterized on the basis of spectral data and metal analysis. Metal to ligand stoichiometry of 1: 3/2 and 1: 5/2 has been proposed for the complexes. The relevant infrared bands in the ligands and complexes were used to assign the probable point(s) of coordination. (author)

Encapsulation of ferro- and ferricyanide complexes inside ZSM-5 zeolite synthesized from rice straw: Implications for synthesis of Prussian blue pigment

Energy Technology Data Exchange (ETDEWEB)

Ali, Ibraheem O.; Salama, Tarek M., E-mail: tm_salama@yahoo.com; Thabet, Mohamed S.; El-Nasser, Karam S.; Hassan, Ali M.

2013-06-15

Encapsulation of [Fe(CN){sub 6}]{sup 4−} and [Fe(CN){sub 6}]{sup 3−} complexes in the intracrystalline pores of ZSM-5 zeolite, Fe{sup II}L/Z and Fe{sup III}L/Z respectively, by the zeolite synthesis method was reported. The modified zeolites were characterized by powder XRD, FT-IR and UV–vis spectroscopy. The nitrogen adsorption isotherms allow for the evaluation of pore structure of the complex-modified zeolites, whereas the thermal analysis (TGA/DTA) measurements provide insight into the decomposition products of the immobilized complexes. The modified zeolites exhibited smaller pore volumes and surface areas as compared with those of unpromoted ZSM-5, suggesting the inclusion of iron cyanides inside the interconnecting channels of ZSM-5. While the ferricyanide complex enhanced the formation of highly crystalline zeolite, the ferrocyanide one resulted in a lesser effect. The electronic spectra of the colloidal species developed when Fe{sup III}L/Z brought in contact with an aqueous solution of [Fe(CN){sub 6}]{sup 3−} exhibit absorptions attributed to CN{sup −} → iron charge-transfer. New bands at 294 and 319 nm due to d–d transitions of Fe{sup III} tetrahedral monomeric moieties were emitted concurrently under successive adsorption of [Fe(CN){sub 6}]{sub aq}{sup 3−} over Fe{sup III}L/Z, along with a broad band at 555 nm assigned to polymeric [Fe{sup II}–C–N–Fe{sup III}] of Prussian blue (PB). The FT-IR spectra of Fe{sup III/II}L/Z devoted to the adsorption of an aqueous solution of [Fe(CN){sub 6}]{sup 3−} showed a band at 2092 cm{sup −1} assigned to the C–N stretch in the Fe{sup II}–CN–Fe{sup III} linkages. The vibrations attributable to Fe–O–Si bonding along with hydrocarbon and nitroprusside appeared only in the spectrum of Fe{sup III}L/Z, thus was found to be strong evidence for the mutual interaction between [Fe(CN){sub 6}]{sup 3−} and the latter sample. - Highlights: • We synthesized ferrous and ferric cyanide

High-Performance solar-blind flexible Deep-UV photodetectors based on quantum dots synthesized by femtosecond-laser ablation

KAUST Repository

Mitra, Somak; Aravindh, Assa; Das, Gobind; Pak, Yusin; Ajia, Idris A.; Loganathan, Kalaivanan; Di Fabrizio, Enzo M.; Roqan, Iman S.

2018-01-01

-performance flexible DUV photodetectors operating at ambient conditions based on quantum dots (QDs) synthesized by femtosecond-laser ablation in liquid (FLAL) technique. Our method is facile without complex chemical procedures, which allows large-scale cost

-Heterocyclic Carbene Complexes of Mineral Acids

KAUST Repository

Brill, Marcel; Nahra, Fady; Gó mez-Herrera, Alberto; Zinser, Caroline; Cordes, David B.; Slawin, Alexandra M. Z.; Nolan, Steven P.

2016-01-01

We have synthesized and characterized new gold-N-heterocyclic carbene (NHC) complexes derived from the deprotonation of mineral acids. The use of sulfuric acid was a particularly interesting case. These complexes were tested in known gold-catalyzed reactions, such as the hydration of alkynes and the Meyer–Schuster rearrangement. They proved to be highly efficient in both reactions.

-Heterocyclic Carbene Complexes of Mineral Acids

KAUST Repository

Brill, Marcel

2016-11-08

We have synthesized and characterized new gold-N-heterocyclic carbene (NHC) complexes derived from the deprotonation of mineral acids. The use of sulfuric acid was a particularly interesting case. These complexes were tested in known gold-catalyzed reactions, such as the hydration of alkynes and the Meyer–Schuster rearrangement. They proved to be highly efficient in both reactions.

Syntheses, structures, and properties of imidazolate-bridged Cu(II)-Cu(II) and Cu(II)-Zn(II) dinuclear complexes of a single macrocyclic ligand with two hydroxyethyl pendants.

Science.gov (United States)

Li, Dongfeng; Li, Shuan; Yang, Dexi; Yu, Jiuhong; Huang, Jin; Li, Yizhi; Tang, Wenxia

2003-09-22

The imidazolate-bridged homodinuclear Cu(II)-Cu(II) complex, [(CuimCu)L]ClO(4).0.5H(2)O (1), and heterodinuclear Cu(II)-Zn(II) complex, [(CuimZnL(-)(2H))(CuimZnL(-)(H))](ClO(4))(3) (2), of a single macrocyclic ligand with two hydroxyethyl pendants, L (L = 3,6,9,16,19,22-hexaaza-6,19-bis(2-hydroxyethyl)tricyclo[22,2,2,2(11,14)]triaconta-1,11,13,24,27,29-hexaene), have been synthesized as possible models for copper-zinc superoxide dismutase (Cu(2),Zn(2)-SOD). Their crystal structures analyzed by X-ray diffraction methods have shown that the structures of the two complexes are markedly different. Complex 1 crystallizes in the orthorhombic system, containing an imidazolate-bridged dicopper(II) [Cu-im-Cu](3+) core, in which the two copper(II) ions are pentacoordinated by virtue of an N4O environment with a Cu.Cu distance of 5.999(2) A, adopting the geometry of distorted trigonal bipyramid and tetragonal pyramid, respectively. Complex 2 crystallizes in the triclinic system, containing two similar Cu-im-Zn cores in the asymmetric unit, in which both the Cu(II) and Zn(II) ions are pentacoordinated in a distorted trigonal bipyramid geometry, with the Cu.Zn distance of 5.950(1)/5.939(1) A, respectively. Interestingly, the macrocyclic ligand with two arms possesses a chairlike (anti) conformation in complex 1, but a boatlike (syn) conformation in complex 2. Magnetic measurements and ESR spectroscopy of complex 1 have revealed the presence of an antiferromagnetic exchange interaction between the two Cu(II) ions. The ESR spectrum of the Cu(II)-Zn(II) heterodinuclear complex 2 displayed a typical signal for mononuclear trigonal bipyramidal Cu(II) complexes. From pH-dependent ESR and electronic spectroscopic studies, the imidazolate bridges in the two complexes have been found to be stable over broad pH ranges. The cyclic voltammograms of the two complexes have been investigated. Both of the two complexes can catalyze the dismutation of superoxide and show rather high activity.

Syntheses and radiolabeling of cysteine-oximes and pharmacological behaviour of their 99mTc complexes

International Nuclear Information System (INIS)

Kothari, Kanchan; Banerjee, Sharmila; Sarma, H.D.; Pillai, M.R.A.

2000-01-01

Synthesis of two novel ligands using 2-oximino-butan-3-one and L-ethyl cysteinate is described. The synthetic procedure involved the formation of Schiff's base by the condensation of the amino group of L-ethyl cysteinate with the carbonyl group of 2-oximino-butan-3-one to provide the ligand I, N'(butan-2-enyl-3-oximino)ethyl cysteinate, followed by reduction of the Schiff's base with sodium borohydride to ligand II, N'(3-oximinobutyl)ethyl cysteinate. The ligands were characterised by NMR spectroscopy. Complexation studies with 99m Tc were carried out using stannous tartrate as the reducing agent. The complexes were characterised by paper chromatography, thin layer chromatography and paper electrophoresis techniques. The complexes are formed in high yields when the reactions were carried out at pH 7-9. The 99m Tc complex with ligand I is formed instantaneously while the 99m Tc complex with ligand II is formed at a slower rate. The complexes were found to be neutral but the lipophilicity of the complex with ligand I was higher than that of the complex of ligand II. The stability of the complex with ligand I was relatively poor as compared to that of the complex with ligand II. Biodistribution studies of the 99m Tc complexes of ligand I and II showed rapid blood clearance with hepatobiliary uptake. Renal excretion of the complex of ligand II was more than that observed for the complex of ligand I. The complexes did not show significant uptake in brain in spite of their favourable properties such as neutrality, lipophilicity and structural similarity with both ECD and HMPAO

Rationalization of Anomalous Pseudocontact Shifts and Their Solvent Dependence in a Series of C3-Symmetric Lanthanide Complexes.

Science.gov (United States)

Vonci, Michele; Mason, Kevin; Suturina, Elizaveta A; Frawley, Andrew T; Worswick, Steven G; Kuprov, Ilya; Parker, David; McInnes, Eric J L; Chilton, Nicholas F

2017-10-11

Bleaney's long-standing theory of magnetic anisotropy has been employed with some success for many decades to explain paramagnetic NMR pseudocontact shifts, and has been the subject of many subsequent approximations. Here, we present a detailed experimental and theoretical investigation accounting for the anomalous solvent dependence of NMR shifts for a series of lanthanide(III) complexes, namely [LnL 1 ] (Ln = Eu, Tb, Dy, Ho, Er, Tm, and Yb; L 1 : 1,4,7-tris[(6-carboxypyridin-2-yl)methyl]-1,4,7-triazacyclononane), taking into account the effect of subtle ligand flexibility on the electronic structure. We show that the anisotropy of the room temperature magnetic susceptibility tensor, which in turn affects the sign and magnitude of the pseudocontact chemical shift, is extremely sensitive to minimal structural changes in the first coordination sphere of L 1 . We show that DFT structural optimizations do not give accurate structural models, as assessed by the experimental chemical shifts, and thus we determine a magnetostructural correlation and employ this to evaluate the accurate solution structure for each [LnL 1 ]. This approach allows us to explain the counterintuitive pseudocontact shift behavior, as well as a striking solvent dependence. These results have important consequences for the analysis and design of novel magnetic resonance shift and optical emission probes that are sensitive to the local solution environment and polarity.

Preparation, spectroscopic studies and X-ray structure of homobinuclear lanthanide(III complexes derived from 2,6-diformyl-4-chlorophénol-bis-(2’-hydroxy-benzoylhydrazone

Directory of Open Access Journals (Sweden)

Pepe Marcel Haba

2006-06-01

Full Text Available Reaction of the 2,6-diformyl-4-chlorophenol-bis-(2'-hydroxy-benzoylhydrazone with Ln(NO33.nH2O (n = 5 or 6 and Ln = Y, La, Ce, Pr, Nd, Sm, Gd, Dy, Er and Yb produces homobinuclear complexes. These complexes have been characterized by analysis, molar conductance, magnetic measurements, infrared spectral studies and X-ray diffraction. The analytical data showed 1:3 (metal:ligand stoichiometry. Molar conductance measurements in dmf indicate 1:3 electrolytes in all cases. Magnetic moment values are close proximity of the Van Vleck values. IR studies suggest the coordination of the ligand is through the azomethine, the phenolic oxygen atom and the carbonyl oxygen of the hydrazonic moiety. The nitrate ion is also found to be ionic in all the complexes. An X-ray structure determination of [C66H48N12O15Cl3Er2]Cl2NO3.5H2O confirms the conclusion from the spectroscopic studies and show that the erbium is at the centre of a tricapped trigonal prism with coordination number nine. In all the complexes the lanthanide ions have substantially similar coordination.

Composites comprising biologically-synthesized nanomaterials

Science.gov (United States)

Curran, Seamus; Dias, Sampath; Blau, Werner; Wang, Jun; Oremland, Ronald S; Baesman, Shaun

2013-04-30

The present disclosure describes composite materials containing a polymer material and a nanoscale material dispersed in the polymer material. The nanoscale materials may be biologically synthesized, such as tellurium nanorods synthesized by Bacillus selenitireducens. Composite materials of the present disclosure may have optical limiting properties and find use in optical limiting devices.

Low-Entropy States of Neutral Atoms in Polarization-Synthesized Optical Lattices.

Science.gov (United States)

Robens, Carsten; Zopes, Jonathan; Alt, Wolfgang; Brakhane, Stefan; Meschede, Dieter; Alberti, Andrea

2017-02-10

We create low-entropy states of neutral atoms by utilizing a conceptually new optical-lattice technique that relies on a high-precision, high-bandwidth synthesis of light polarization. Polarization-synthesized optical lattices provide two fully controllable optical lattice potentials, each of them confining only atoms in either one of the two long-lived hyperfine states. By employing one lattice as the storage register and the other one as the shift register, we provide a proof of concept using four atoms that selected regions of the periodic potential can be filled with one particle per site. We expect that our results can be scaled up to thousands of atoms by employing an atom-sorting algorithm with logarithmic complexity, which is enabled by polarization-synthesized optical lattices. Vibrational entropy is subsequently removed by sideband cooling methods. Our results pave the way for a bottom-up approach to creating ultralow-entropy states of a many-body system.

Synthesizing biomolecule-based Boolean logic gates.

Science.gov (United States)

Miyamoto, Takafumi; Razavi, Shiva; DeRose, Robert; Inoue, Takanari

2013-02-15

One fascinating recent avenue of study in the field of synthetic biology is the creation of biomolecule-based computers. The main components of a computing device consist of an arithmetic logic unit, the control unit, memory, and the input and output devices. Boolean logic gates are at the core of the operational machinery of these parts, and hence to make biocomputers a reality, biomolecular logic gates become a necessity. Indeed, with the advent of more sophisticated biological tools, both nucleic acid- and protein-based logic systems have been generated. These devices function in the context of either test tubes or living cells and yield highly specific outputs given a set of inputs. In this review, we discuss various types of biomolecular logic gates that have been synthesized, with particular emphasis on recent developments that promise increased complexity of logic gate circuitry, improved computational speed, and potential clinical applications.

Synthesizing Biomolecule-based Boolean Logic Gates

Science.gov (United States)

Miyamoto, Takafumi; Razavi, Shiva; DeRose, Robert; Inoue, Takanari

2012-01-01

One fascinating recent avenue of study in the field of synthetic biology is the creation of biomolecule-based computers. The main components of a computing device consist of an arithmetic logic unit, the control unit, memory, and the input and output devices. Boolean logic gates are at the core of the operational machinery of these parts, hence to make biocomputers a reality, biomolecular logic gates become a necessity. Indeed, with the advent of more sophisticated biological tools, both nucleic acid- and protein-based logic systems have been generated. These devices function in the context of either test tubes or living cells and yield highly specific outputs given a set of inputs. In this review, we discuss various types of biomolecular logic gates that have been synthesized, with particular emphasis on recent developments that promise increased complexity of logic gate circuitry, improved computational speed, and potential clinical applications. PMID:23526588

Complexes of uranyl nitrate with 2,6-pyridinedicarboxamides: synthesis, crystal structure, and DFT study

Energy Technology Data Exchange (ETDEWEB)

Alyapyshev, Mikhail; Babain, Vasiliy [ITMO University, 49, Kronverksky pr., 197101, St. Petersburg (Russian Federation); ThreeArc Mining Ltd., 5, Stary Tolmachevskiy per., 115184, Moscow (Russian Federation); Tkachenko, Lyudmila; Lumpov, Alexander [Khlopin Radium Institute, 28, 2nd Murinskiy pr., 194021, St. Petersburg (Russian Federation); Gurzhiy, Vladislav; Zolotarev, Andrey; Dar' in, Dmitriy [St. Petersburg State University, 7-9, Universitetskaya nab., 199034, St. Petersburg (Russian Federation); Ustynyuk, Yuriy; Gloriozov, Igor [M.V. Lomonosov Moscow State University, 119991, Moscow (Russian Federation); Paulenova, Alena [Department of Nuclear Engineering, Oregon State University, Corvallis, OR (United States)

2017-05-04

Two complexes of uranyl nitrate with N,N,N',N'-tetrabutyl-2,6-pyridinedicarboxamide (TBuDPA) and N,N'-diethyl-N,N'-diphenyl-2,6-pyridinedicarboxamide (EtPhDPA) were synthesized and studied. The complex of tetraalkyl-2,6-pyridinedicarboxamide with metal nitrate was synthesized for the first time. XRD analysis revealed the different type of complexation: a 1:1 metal:ligand complex for EtPhDPA and complex with polymeric structure for TBuDPA. The quantum chemical calculations (DFT) confirm that both ligands form the most stable complexes that match the minimal values pre-organization energy of the ligands. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

Thin films of molecular materials synthesized from fisher's carbene ferrocenyl: Film formation and electrical properties

International Nuclear Information System (INIS)

Sanchez-Vergara, M.E.; Ortiz, A.; Alvarez-Toledano, C.; Moreno, A.; Alvarez, J.R.

2008-01-01

The synthesis of materials from Fisher's carbene ferrocenyl of the elements chromium, molybdenum and tungsten was carried out. The Fisher's compounds that were synthesized included the following combinations of two different metallic atoms: iron with chromium, iron with molybdenum and iron with tungsten. The molecular solids' preparation was done in electro-synthesis cells with platinum electrodes. Thin films were prepared by vacuum thermal evaporation on quartz substrates and crystalline silicon wafers. Pellets and thin films from these compounds were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, energy-dispersive spectroscopy, atomic force microscopy and ellipsometry. The powder and thin films synthesized from these materials show the same intra-molecular bonds shown by infrared spectroscopy results, suggesting that thermal evaporation does not alter these bonds in spite of the thin films being amorphous, in contrast with other bimetallic complexes where material decomposition occurs. The differences in the conductivity values of the prepared films are very small, so they may be attributed to the different metallic ions employed in each case. The tungsten complex exhibits a higher conductivity than the molybdenum and chromium complexes at room temperature. Electrical conductivity values found for thin films are higher than for pellets made of the same molecular materials

γ-Irradiation and characterization of synthesized methoxybenzylpyrimidine formimidate Schiff-base and some metal-complex derivatives

Directory of Open Access Journals (Sweden)

R.O. Aly

2016-09-01

The magnetic properties together with the UV–Vis reposted data revealed the octahedral coordination of the Zn- and La-complex and the tetragonal distortion geometry of the Cu-complex. The La-complexes revealed only moderate inhibition against the Gram-negative Escherichia coli, whereas the Zn-complex revealed significant inhibition. The latter showed also similar effect against the Gram-positive Bacillus subtilis and Streptococcus pyogens (ATCC-19615.

Tris-diamine-derived transition metal complexes of flurbiprofen as ...

African Journals Online (AJOL)

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butyrylcholinesterase (BChE) inhibitory activities. Method: Tris-diamine-derived transition metal complexes of Co(II), Ni(II), and Mn(II) were synthesized and characterized ... Conductance measurements indicated that diamine-derived metal complexes of ..... contributes to enhanced biological activity, and provides novel ...

Meta-analysis and other approaches for synthesizing structured and unstructured data in plant pathology.

Science.gov (United States)

Scherm, H; Thomas, C S; Garrett, K A; Olsen, J M

2014-01-01

The term data deluge is used widely to describe the rapidly accelerating growth of information in the technical literature, in scientific databases, and in informal sources such as the Internet and social media. The massive volume and increased complexity of information challenge traditional methods of data analysis but at the same time provide unprecedented opportunities to test hypotheses or uncover new relationships via mining of existing databases and literature. In this review, we discuss analytical approaches that are beginning to be applied to help synthesize the vast amount of information generated by the data deluge and thus accelerate the pace of discovery in plant pathology. We begin with a review of meta-analysis as an established approach for summarizing standardized (structured) data across the literature. We then turn to examples of synthesizing more complex, unstructured data sets through a range of data-mining approaches, including the incorporation of 'omics data in epidemiological analyses. We conclude with a discussion of methodologies for leveraging information contained in novel, open-source data sets through web crawling, text mining, and social media analytics, primarily in the context of digital disease surveillance. Rapidly evolving computational resources provide platforms for integrating large and complex data sets, motivating research that will draw on new types and scales of information to address big questions.

Design of a 2.4-GHz CMOS monolithic fractional-N frequency synthesizer

Science.gov (United States)

Shu, Keliu

The wireless communication technology and market have been growing rapidly since a decade ago. The high demand market is a driving need for higher integration in the wireless transceivers. The trend is to achieve low-cost, small form factor and low power consumption. With the ever-reducing feature size, it is becoming feasible to integrate the RF front-end together with the baseband in the low-cost CMOS technology. The frequency synthesizer is a key building block in the RF front-end of the transceivers. It is used as a local oscillator for frequency translation and channel selection. The design of a 2.4-GHz low-power frequency synthesizer in 0.35mum CMOS is a challenging task mainly due to the high-speed prescaler. In this dissertation, a brief review of conventional PLL and frequency synthesizers is provided. Design techniques of a 2.4-GHz monolithic SigmaDelta fractional-N frequency synthesizer are investigated. Novel techniques are proposed to tackle the speed and integration bottlenecks of high-frequency PLL. A low-power and inherently glitch-free phase-switching prescaler and an on-chip loop filter with capacitance multiplier are developed. Compared with the existing and popular dual-path topology, the proposed loop filter reduces circuit complexity and its power consumption and noise are negligible. Furthermore, a third-order three-level digital SigmaDelta modulator topology is employed to reduce the phase noise generated by the modulator. Suitable PFD and charge-pump designs are employed to reduce their nonlinearity effects and thus minimize the folding of the SigmaDelta modulator-shaped phase noise. A prototype of the fractional-N synthesizer together with some standalone building blocks is designed and fabricated in TSMC 0.35mum CMOS through MOSIS. The prototype frequency synthesizer and standalone prescaler and loop filter are characterized. The feasibility and practicality of the proposed prescaler and loop filter are experimentally verified.

Synthesis and characterization of thorium(IV) and uranium(IV) complexes with Schiff bases

Energy Technology Data Exchange (ETDEWEB)

Radoske, Thomas; Maerz, Juliane; Kaden, Peter; Patzschke, Michael; Ikeda-Ohno, Atsushi [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Chemistry of the F-Elements

2017-06-01

We report herein the synthesis and characterization of several imine complexes of tetravalent thorium (Th(IV)) and uranium (U(IV)). The ligands investigated in this study are a Schiff base type, including the well-known salen ligand (H{sub 2}Le, Fig. 1). The complexation in solution was investigated by NMR measurements indicating paramagnetic effects of unpaired f-electrons of U(IV) on the ligand molecule. We also determined the solid-state molecular structures of the synthesized complexes by single crystal X-ray diffraction. The synthesized complexes show an eight-fold coordination geometry around the actinide center surrounded by two tetradentate ligands with 2N- and 2O-donor atoms.

ADP-ribosyl-N₃: A Versatile Precursor for Divergent Syntheses of ADP-ribosylated Compounds.

Science.gov (United States)

Li, Lingjun; Li, Qianqian; Ding, Shengqiang; Xin, Pengyang; Zhang, Yuqin; Huang, Shenlong; Zhang, Guisheng

2017-08-14

Adenosine diphosphate-ribose (ADP-ribose) and its derivatives play important roles in a series of complex physiological procedures. The design and synthesis of artificial ADP-ribosylated compounds is an efficient way to develop valuable chemical biology tools and discover new drug candidates. However, the synthesis of ADP-ribosylated compounds is currently difficult due to structural complexity, easily broken pyrophosphate bond and high hydrophilicity. In this paper, ADP-ribosyl-N₃ was designed and synthesized for the first time. With ADP-ribosyl-N₃ as the key precursor, a divergent post-modification strategy was developed to prepare structurally diverse ADP-ribosylated compounds including novel nucleotides and peptides bearing ADP-ribosyl moieties.

A lanthanide complex with dual biosensing properties: CEST (chemical exchange saturation transfer) and BIRDS (biosensor imaging of redundant deviation in shifts) with europium DOTA-tetraglycinate.

Science.gov (United States)

Coman, Daniel; Kiefer, Garry E; Rothman, Douglas L; Sherry, A Dean; Hyder, Fahmeed

2011-12-01

Responsive contrast agents (RCAs) composed of lanthanide(III) ion (Ln3R) complexes with a variety of1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetate (DOTA4S) derivatives have shown great potential as molecular imaging agents for MR. A variety of LnDOTA–tetraamide complexes have been demonstrated as RCAs for molecular imaging using chemical exchange saturation transfer (CEST). The CEST method detects proton exchange between bulk water and any exchangeable sites on the ligand itself or an inner sphere of bound water that is shifted by a paramagnetic Ln3R ion bound in the core of the macrocycle. It has also been shown that molecular imaging is possible when the RCA itself is observed (i.e. not its effect on bulk water) using a method called biosensor imaging of redundant deviation in shifts (BIRDS). The BIRDS method utilizes redundant information stored in the nonexchangeable proton resonances emanating from the paramagnetic RCA for ambient factors such as temperature and/or pH.Thus, CEST and BIRDS rely on exchangeable and nonexchangeable protons, respectively, for biosensing. We posited that it would be feasible to combine these two biosensing features into the same RCA (i.e. dual CEST and BIRDS properties). A complex between europium(III) ion (Eu3R) and DOTA–tetraglycinate [DOTA–(gly)S4] was used to demonstrate that its CEST characteristics are preserved, while its BIRDS properties are also detectable. The in vitro temperature sensitivity of EuDOTA–(gly)S4 was used to show that qualitative MR contrast with CEST can be calibrated using quantitative MR mapping with BIRDS, thereby enabling quantitative molecular imaging at high spatial resolution.

Dramatic improvement in photostability of luminescent Eu(III) complexes with tetraphenylimidodiphosphinate ligand

International Nuclear Information System (INIS)

Zheng, Wei; Li, Shu-Jing; Li, Cheng-Hui; Zheng, You-Xuan; You, Xiao-Zeng

2014-01-01

In this paper, we synthesized and characterized a new Eu(III) tetraphenylimidodiphosphinate complex with dimethyl sulfoxide (DMSO) as co-ligand. Moreover, we compared the photostability of a series of Eu(III) complexes containing tetraphenylimidodiphosphinate ligands, Eu(tpip) 3 , Eu(tpip) 3 Phen, Eu(tpip) 3 DMSO, with their analogs of 1,3-dibenzoylmethanate, Eu(dbm) 3 ∙2H 2 O, Eu(dbm) 3 Phen, Eu(dbm) 3 (DMSO) 2 . We found that the photostability of the luminescent Eu(III) complexes was significantly improved upon substitution of the 1,3-diketones with tetraphenylimidodiphosphinate ligands. -- Highlights: • We synthesized and characterized a new Eu(III) tetraphenylimidodiphosphinate complexes with dimethyl sulfoxide. • We compared the photostability of Eu(III) complex with tetraphenylimidodiphosphinate and 1,3-dibenzoylmethanate ligands. • The photostability is significantly improved in Eu(III) complexes with tetraphenylimidodiphosphinate ligands

Usefulness of charge-transfer complexation for the assessment of sympathomimetic drugs: Spectroscopic properties of drug ephedrine hydrochloride complexed with some π-acceptors

Science.gov (United States)

Refat, Moamen S.; Ibrahim, Omar B.; Saad, Hosam A.; Adam, Abdel Majid A.

2014-05-01

Recently, ephedrine (Eph) assessment in food products, pharmaceutical formulations, human fluids of athletes and detection of drug toxicity and abuse, has gained a growing interest. To provide basic data that can be used to assessment of Eph quantitatively based on charge-transfer (CT) complexation, the CT complexes of Eph with 7‧,8,8‧-tetracyanoquinodimethane (TCNQ), dichlorodicyanobenzoquinone (DDQ), 1,3-dinitrobenzene (DNB) or tetrabromothiophene (TBT) were synthesized and spectroscopically investigated. The newly synthesized complexes have been characterized via elemental analysis, IR, Raman, 1H NMR, and UV-visible spectroscopy. The formation constant (KCT), molar extinction coefficient (εCT) and other spectroscopic data have been determined using the Benesi-Hildebrand method and its modifications. The sharp, well-defined Bragg reflections at specific 2θ angles have been identified from the powder X-ray diffraction patterns. Thermal decomposition behavior of these complexes was also studied, and their kinetic thermodynamic parameters were calculated with Coats-Redfern and Horowitz-Metzger equations.

Decentralized control of complex systems

CERN Document Server

Siljak, Dragoslav D

2011-01-01

Complex systems require fast control action in response to local input, and perturbations dictate the use of decentralized information and control structures. This much-cited reference book explores the approaches to synthesizing control laws under decentralized information structure constraints.Starting with a graph-theoretic framework for structural modeling of complex systems, the text presents results related to robust stabilization via decentralized state feedback. Subsequent chapters explore optimization, output feedback, the manipulative power of graphs, overlapping decompositions and t

Interaction between serum albumins and sonochemically synthesized cadmium sulphide nanoparticles: a spectroscopic study

International Nuclear Information System (INIS)

Naveenraj, Selvaraj; Asiri, Abdullah M.; Anandan, Sambandam

2013-01-01

Cadmium Sulphide nanoparticles approximately 5–10 nm in size range were synthesized by sonochemical technique, which follows acoustic cavitation phenomenon and generates nanoparticles with a smaller size range and higher surface area. The in vitro binding interaction of these sonochemically synthesized CdS nanoparticles with serum albumins (SA) were investigated using UV–Vis absorption, fluorescence and circular dichroism (CD) spectroscopic techniques since CdS nanoparticles has biological applications such as cellular labelling and deep-tissue imaging. UV–Vis absorption and fluorescence studies confirm that CdS nanoparticles bind with SA through ground state complex formation (static quenching mechanism). The results suggest that sonochemically synthesized CdS nanoparticles interact with HSA more than that of BSA and these nanoparticles can be easily transported and rapidly released to the targets by serum albumins. CD studies confirmed the conformational change of serum albumins on the interaction of CdS nanoparticles.Graphical AbstractThis paper investigates the in vitro binding interaction of Cadmium Sulphide (CdS) nanoparticles with serum albumins (HSA and BSA) using the UV-vis, steady-state fluorescence, time-resolved fluorescence, synchronous fluorescence and circular dichroism (CD) spectral techniques.

The preparation and use of metal salen complexes derived from cyclobutane diamine

Science.gov (United States)

Patil, Smita

The helix is an important chiral motif in nature, there is increasing development in field of helical transition metal complexes and related supramolecular structures. Hence, the goals of this work are to apply the principles of helicity in order to produce metal complexes with predictable molecular shapes and to study their properties as asymmetric catalysts. Computational studies suggest that the (1R,2 R)-cyclobutyldiamine unit can produce highly twisted salen complexes with a large energy barrier between the M and P helical forms. To test this prediction, the tartrate salt of (1R,2R)-cyclobutyldiamine was synthesized and condensed with a series of saliclaldehydes to produce novel salen ligands. The salicylaldehydes chosen have extended phenanthryl or benz[a]anthryl sidearms to encourage formation of helical coordination complexes. These ligands were metallated with zinc, iron and manganese salts to produce salen metal complexes which were characterized by NMR analysis, high-resolution mass spectrometry, and IR spectroscopy. A second ligand type, neutral bis(pyridine-imine) has also been synthesized from (1R,2R)-cyclobutyldiamine and quinolylaldehydes. The synthesis of bis(pyridine-imine) ligands was conducted using greener method, solvent assisted grinding. These ligands, in-situ with nickel metal salts, showed good catalytic activity for asymmetric Diels-Alder reactions. The third ligand type studied was chiral acid-functionalized Schiff-base ligands. These were synthesized by the condensation of 3-formyl-5-methyl salicylic acid and (1R,2R)-cyclobutyldiamine. With this type of ligand, there is possibility of producing both mono and dinuclear metal complexes. In our studies, we were only able to synthesize mononuclear complexs. These were tested as catalysts for asymmetric direct Mannich-type reaction, but were found to be ineffective.

Synthesizing lattice structures in phase space

International Nuclear Information System (INIS)

Guo, Lingzhen; Marthaler, Michael

2016-01-01

In one dimensional systems, it is possible to create periodic structures in phase space through driving, which is called phase space crystals (Guo et al 2013 Phys. Rev. Lett. 111 205303). This is possible even if for particles trapped in a potential without periodicity. In this paper we discuss ultracold atoms in a driven optical lattice, which is a realization of such a phase space crystals. The corresponding lattice structure in phase space is complex and contains rich physics. A phase space lattice differs fundamentally from a lattice in real space, because its coordinate system, i.e., phase space, has a noncommutative geometry, which naturally provides an artificial gauge (magnetic) field. We study the behavior of the quasienergy band structure and investigate the dissipative dynamics. Synthesizing lattice structures in phase space provides a new platform to simulate the condensed matter phenomena and study the intriguing phenomena of driven systems far away from equilibrium. (paper)

Syntheses and characterizations of secondary Pb-O bonding supported Pb(II)-sulfonate complexes

Science.gov (United States)

Huang, Guo-Zhen; Zou, Xin; Zhu, Zhi-Biao; Deng, Zhao-Peng; Huo, Li-Hua; Gao, Shan

2018-06-01

The reaction of Pb(II) salts and mono- or disulfonates leads to the formation of eight new Pb(II)-mono/disulfonate complexes, [Pb(L1)(H2O)]2 (1), [Pb4(L2)2(AcO)2]n·5nH2O (2), [Pb(L3)(H2O)]2 (3), [Pb(HL4)(H2O)2]n·nH2O (4), [Pb(HL5)(H2O)2]n·2nH2O (5), [Pb(H2L6)(H2O)]n·nDMF·2nH2O (6), [Pb2(H3L7)4(H2O)6]·2H2O (7) and [Pb(H2L7)(H2O)]n·nH2O (8) (H2L1= 2-hydroxy-5-methyl-benzenesulfonic acid, H3L2= 2-hydroxyl-5-methyl- 1,3-benzenedisulfonic acid, H2L3= 2-hydroxy-5-nitro-benzenesulfonic acid, H3L4= 2-hydroxyl-5-bromo-1,3- benzenedisulfonic acid, H3L5= 2-hydroxyl-5-carboxyl-benzenesulfonic acid, H4L6= 2,5-dihydroxyl-3-carboxyl- benzenesulfonic acid, H4L7= 2,4-dihydroxyl-5-carboxyl-benzenesulfonic acid, DMF = N,N'-dimethyl-formamide, AcO- = acetate), which have been characterized by elemental analysis, IR, TG, PL, powder and single-crystal X-ray diffraction. In view of the primary Pb-O bonds, these eight complexes exhibit diverse dinuclear (1, 3 and 7), helical chain (4), wave-like chain (5), linear chain (6), zigzag chain (8) and layer structure (2), in which the Pb(II) cations present different hemi-directed geometries. Taking the secondary Pb-O bonds into account, chain structure for complex 7, layer motifs for complexes 1 and 3-6, as well as 3-D framework for complex 8 are observed with Pb(II) cations showing more intricate holo-directed geometries. The various coordination modes of these seven different mono/disulfonate anions are responsible for the formation of these multiple structures. Furthermore, the introduction of hydroxyl and carboxyl groups increases the coordination ability of sulfonate to the p-block metal cation. Luminescent analyses indicate that complex 7 presents purple emission at 395 nm at room temperature.

Highly Luminescent, Water-Soluble Lanthanide Fluorobenzoates: Syntheses, Structures and Photophysics, Part I: Lanthanide Pentafluorobenzoates.

Science.gov (United States)

Kalyakina, Alena S; Utochnikova, Valentina V; Bushmarinov, Ivan S; Ananyev, Ivan V; Eremenko, Igor L; Volz, Daniel; Rönicke, Franziska; Schepers, Ute; Van Deun, Rik; Trigub, Alexander L; Zubavichus, Yan V; Kuzmina, Natalia P; Bräse, Stefan

2015-12-01

Highly luminescent, photostable, and soluble lanthanide pentafluorobenzoates have been synthesized and thoroughly characterized, with a focus on Eu(III) and Tb(III) complexes as visible emitters and Nd(III) , Er(III) , and Yb(III) complexes as infrared emitters. Investigation of the crystal structures of the complexes in powder form and as single crystals by using X-ray diffraction revealed five different structural types, including monomeric, dimeric, and polymeric. The local structure in different solutions was studied by using X-ray absorption spectroscopy. The photoluminescence quantum yields (PLQYs) of terbium and europium complexes were 39 and 15 %, respectively; the latter value was increased almost twice by using the heterometallic complex [Tb0.5 Eu0.5 (pfb)3 (H2 O)] (Hpfb=pentafluorobenzoic acid). Due to the effectively utilized sensitization strategy (pfb)(-) →Tb→Eu, a pure europium luminescence with a PLQY of 29 % was achieved. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Synthesis, characterization and biological assay of Salicylaldehyde Schiff base Cu(II) complexes and their precursors

Science.gov (United States)

Iftikhar, Bushra; Javed, Kanwal; Khan, Muhammad Saif Ullah; Akhter, Zareen; Mirza, Bushra; Mckee, Vickie

2018-03-01

Three new Schiff base ligands were synthesized by the reaction of Salicylaldehyde with semi-aromatic diamines, prepared by the reduction of corresponding dinitro-compounds, and were further used for the formation of complexes with Cu(II) metal ion. The structural features of the synthesized compounds were confirmed by their physical properties and infrared, electronic and NMR spectroscopic techniques. The studies revealed that the synthesized Schiff bases existed as tetradentate ligands and bonded to the metal ion through the phenolic oxygen and azomethine nitrogen. One of the dinitro precursors was also analyzed by single crystal X-ray crystallography, which showed that it crystallizes in monoclinic system with space group P2/n. The thermal behavior of the Cu(II) complexes was determined by thermogravimetric analysis (TGA) and kinetic parameters were evaluated from the data. Schiff base ligands, their precursors and metal complexes were also screened for antibacterial, antifungal, antitumor, Brine shrimp lethality, DPPH free radical scavenging and DNA damage assays. The results of these analyses indicated the substantial potential of the synthesized Schiff bases, their precursors and Cu(II) complexes in biological field as future drugs.

Syntheses and a Solid State Structure of a Dinuclear Molybdenum(V Complex with Pyridine

Directory of Open Access Journals (Sweden)

Jon Zubieta

2010-01-01

Full Text Available A mononuclear complex [MoOCl4(H2O]− readily forms a metal−metal bonded {Mo2O4}2+ core. A high content of pyridine in the reaction mixture prevents further aggregation of dinuclear cores into larger clusters and a neutral, dinuclear complex with the [Mo2O4Cl2(Py4] composition is isolated as a product. Solid state structures of two compounds containing this complex, [Mo2O4Cl2(Py4]·2.25Py (1 and [Mo2O4Cl2(Py4]·1.5PyHCl (2, were investigated by X-ray crystallography.

Ni(II) complexes of arginine Schiff-bases and its interaction with DNA

Energy Technology Data Exchange (ETDEWEB)

Sallam, S.A., E-mail: shehabsallam@yahoo.com [Chemistry Department, Faculty of Science, Suez Canal University, Isamilia (Egypt); Abbas, A.M. [Chemistry Department, Faculty of Science, Suez Canal University, Isamilia (Egypt)

2013-04-15

Ni(II) complexes with Schiff-bases obtained by condensation of arginine with salicylaldehyde; 2,3-; 2,4-; 2,5-dihydroxybenzaldehyde and o-hydroxynaphthaldehyde have been synthesized using the template method in ethanol or ammonia media. They were characterized by elemental analyses, conductivity measurements, magnetic moment, UV, IR and {sup 1}H NMR spectra as well as thermal analysis (TG, DTG and DTA). The Schiff-bases are dibasic tridentate donors and the complexes have diamagnetic square planar and octahedral structures. The complexes decompose in three steps where kinetic and thermodynamic parameters of the decomposition steps were computed. The interactions of the formed complexes with FM-DNA were monitored by UV and fluorescence spectroscopy. -- Highlights: ► Arginine Schiff-bases and their nickel(II) complexes have been synthesized. ► Magnetic and spectral data show diamagnetic square planar and octahedral complexes. ► The complexes thermally decompose in three stages. Interaction with FM-DNA shows hyperchromism with blue shift.

Ni(II) complexes of arginine Schiff-bases and its interaction with DNA

International Nuclear Information System (INIS)

Sallam, S.A.; Abbas, A.M.

2013-01-01

Ni(II) complexes with Schiff-bases obtained by condensation of arginine with salicylaldehyde; 2,3-; 2,4-; 2,5-dihydroxybenzaldehyde and o-hydroxynaphthaldehyde have been synthesized using the template method in ethanol or ammonia media. They were characterized by elemental analyses, conductivity measurements, magnetic moment, UV, IR and 1 H NMR spectra as well as thermal analysis (TG, DTG and DTA). The Schiff-bases are dibasic tridentate donors and the complexes have diamagnetic square planar and octahedral structures. The complexes decompose in three steps where kinetic and thermodynamic parameters of the decomposition steps were computed. The interactions of the formed complexes with FM-DNA were monitored by UV and fluorescence spectroscopy. -- Highlights: ► Arginine Schiff-bases and their nickel(II) complexes have been synthesized. ► Magnetic and spectral data show diamagnetic square planar and octahedral complexes. ► The complexes thermally decompose in three stages. Interaction with FM-DNA shows hyperchromism with blue shift

Cadmium complexes with 1,2-dimethylbenzimidazole

Energy Technology Data Exchange (ETDEWEB)

Slyusarenko, K F; Artemenko, M V; Pokhodnya, G A [Kievskij Tekhnologicheskij Inst. Pishchevoj Promyshlennosti (Ukrainian SSR)

1982-02-01

New coordination complexes of Cd(2) with 1, 2 - dimethylbenzimidazole (DMBI) of the composition DMBIxCdX/sub 2/, where X=Cl, Br, I and 2DMBIxCdX/sub 2/, where X=NO/sub 3/, CH/sub 3/COO, SCN as well as acido-complexes of the composition (DMBIH)xCdX/sub 4/ (X=Cl, Br) are synthesized. IR-spectra, diffraction diagrams and curves of radial distribution of atomic density for coordination halides and for the rhodanide complex are investigated. Conclusions on individuality and structure of the compounds obtained are made.

Synthesis of Fe–Li–Cr Multinuclear Complexes as Molecular Magnet Materials

Directory of Open Access Journals (Sweden)

Iis Siti Jahro

2008-03-01

Full Text Available Multinuclear complexes have received considerable interest as molecular magnet materials. Up to now, several complex compounds based on bidentate ligand 2,2’ bipyridine have been synthesized. In this research, the Fe-Li-Cr multinuclear complexes with derivative 2’2- bipyridine ligands: 2-(2’-pyridylquinoline(pq, 2,2’-Pyridil(pdl have been synthesized. The oxalate (ox ligand has also been used as a bridging ligand in these multinuclear complexes. The chemical formula of Li[FeCr(ox2(pq(BF42(H2O2] and [Fe(pdln][LiCr(ox3] complexes have been verified using metal and C, H, N elemental analysis data. The IR spectra in 350 – 4000 cm-1 range exhibit characteristic absorptions, which support the proposed structure of complex. The plausible structure of the compounds has been drawn based on complex formation mechanism. The magnetic susceptibility at room temperature of the pq-complex is about 5.7 BM and of the pdl- complexes are 4.8 and 5.5 BM. These indicated that both spin states of iron(II exist in the multinuclear complexes.

Mixed metal complexes of isoniazid and ascorbic acid: chelation ...

African Journals Online (AJOL)

Novel mixed complexes of isoniazid and ascorbic acid have been synthesized and characterized using infrared, electronic absorption data, elemental analysis, molar conductivity, melting point, thin layer chromatography and solubility. The metal ions involved in the complex formation are Cu2+, Zn2+ and Cd2+. The melting ...

An Experiment on Isomerism in Metal-Amino Acid Complexes.

Science.gov (United States)

Harrison, R. Graeme; Nolan, Kevin B.

1982-01-01

Background information, laboratory procedures, and discussion of results are provided for syntheses of cobalt (III) complexes, I-III, illustrating three possible bonding modes of glycine to a metal ion (the complex cations II and III being linkage/geometric isomers). Includes spectrophotometric and potentiometric methods to distinguish among the…

Alkali metal cation complexation and solvent interactions by robust chromium(III) fluoride complexes

DEFF Research Database (Denmark)

Birk, T.; Magnussen, M.J.; Piligkos, Stergios

2010-01-01

)] have been synthesized from mer-[CrF3(py)(3)] and shown to precipitate sodium salts from solution, of which 3[CrF3(Me(3-)tacn)]center dot 2Na(Bph(4)).solv and 6[CrF3(terpy)]center dot 4Na(Bph(4)).solv have been crystallographically characterized. In these clusters, the neutral fluoride complexes bring...

Unsaturated Mn complex decorated hybrid thioarsenates: Syntheses, crystal structures and physical properties

Energy Technology Data Exchange (ETDEWEB)

Yue, Cheng-Yang [Key Laboratory of Inorganic Chemistry in Universities of Shandong, Department of Chemistry and Chemical Engineering, Jining University, Qufu, Shandong 273155 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou 350002 (China); Lei, Xiao-Wu, E-mail: xwlei_jnu@163.com [Key Laboratory of Inorganic Chemistry in Universities of Shandong, Department of Chemistry and Chemical Engineering, Jining University, Qufu, Shandong 273155 (China); Tian, Ya-Wei; Xu, Jing; Bai, Yi-Qun; Wang, Fei; Zhou, Peng-Fei; Liu, Xiao-Fan [Key Laboratory of Inorganic Chemistry in Universities of Shandong, Department of Chemistry and Chemical Engineering, Jining University, Qufu, Shandong 273155 (China); Yi, Fei-Yan, E-mail: yifeiyan@nbu.edu.cn [Faculty of Materials Science & Chemical Engineering, Ningbo University, Ningbo, Zhejiang 315211 (China)

2016-03-15

The incorporation of unsaturated [Mn(1,2-dap)]{sup 2+}, [Mn(1,2-dap){sub 2}]{sup 2+}, [Mn(2,2-bipy)]{sup 2+} (1,2-dap=1,2-diaminopropane) complex cations with thioarsenate anions of [As{sup III}S{sub 3}]{sup 3−} and [As{sup V}S{sub 4}]{sup 3−} led to three new hybrid manganese thioarsenates, namely, [Mn(1,2-dap)]{sub 2}MnAs{sub 2}S{sub 6} (1), [Mn(1,2-dap){sub 2}]{[Mn(1,2-dap)]_2As_2S_8} (2) and (NH{sub 4})[Mn(2,2-bipy){sub 2}]AsS{sub 4} (3). In compound 1, the unsaturated [Mn(1,2-dap)]{sup 2+} complexes, [MnS{sub 4}]{sup 6−} tetrahedra and [As{sup III}S{sub 3}]{sup 3−} trigonal-pyramids are condensed to form the 1D [Mn(1,2-dap)]{sub 2}MnAs{sub 2}S{sub 6} chain, whereas compound 2 features 2D layer composed of [Mn(1,2-dap)]{sup 2+} and [Mn(1,2-dap){sub 2}]{sup 2+} complexes as well as [As{sup V}S{sub 4}]{sup 3−} tetrahedral units. For compound 3, two [As{sup V}S{sub 4}]{sup 3−} anions bridge two [Mn(2,2-bipy)]{sup 2+} complex cations into a butterfly like {[Mn(2,2-bipy)]_2As_2S_8}{sup 2−} anionic unit. Magnetic measurements indicate the ferrimagnetic behavior for compound 1 and antiferromagnetic (AF) behaviors for compounds 2–3. The UV–vis diffuse-reflectance measurements and electronic structural calculations based on density functional theory (DFT) revealed the title compounds belong to semiconductors with band gaps of 2.63, 2.21, and 1.97 eV, respectively. The narrow band-gap of compound 3 led to the efficient and stable photocatalytic degradation activity over organic pollutant than N-doped P25 under visible light irradiation. - Highlights: Three new hybrid manganese thioarsenates have been prepared and structurally characterized. These hybrid phases feature interesting magnetic and visible light responding photocatalytic properties.

Synthesis of ruthenium (III) complexes with benzimidazole derivatives

International Nuclear Information System (INIS)

Vyas, P.C.; Chahar, Yogesh K.; Garg, Yajula; Seth, Gita

2003-01-01

Complexes of ruthenium with biologically important benzimidazole derivatives, viz. 2-(2'-hydroxyphenyl) benzimidazole (HOPBI), 2-2'- mercaptophenyl) benzimidazole (HSPBI), 2- (2'-hydroxynaphthyl) benzimidazole (HONBI) have been synthesized and characterized. (author)

Syntheses, Characterization, Resolution, and Biological Studies of Coordination Compounds of Aspartic Acid and Glycine

Science.gov (United States)

Akinkunmi, Ezekiel; Ojo, Isaac; Adebajo, Clement; Isabirye, David

2017-01-01

Enantiomerically enriched coordination compounds of aspartic acid and racemic mixtures of coordination compounds of glycine metal-ligand ratio 1 : 3 were synthesized and characterized using infrared and UV-Vis spectrophotometric techniques and magnetic susceptibility measurements. Five of the complexes were resolved using (+)-cis-dichlorobis(ethylenediamine)cobalt(III) chloride, (+)-bis(glycinato)(1,10-phenanthroline)cobalt(III) chloride, and (+)-tris(1,10-phenanthroline)nickel(II) chloride as resolving agents. The antimicrobial and cytotoxic activities of these complexes were then determined. The results obtained indicated that aspartic acid and glycine coordinated in a bidentate fashion. The enantiomeric purity of the compounds was in the range of 22.10–32.10%, with (+)-cis-dichlorobis(ethylenediamine)cobalt(III) complex as the more efficient resolving agent. The resolved complexes exhibited better activity in some cases compared to the parent complexes for both biological activities. It was therefore inferred that although the increase in the lipophilicity of the complexes may assist in the permeability of the complexes through the cell membrane of the pathogens, the enantiomeric purity of the complexes is also of importance in their activity as antimicrobial and cytotoxic agents. PMID:28293149

CAMAC programmable-control frequency synthesizer

International Nuclear Information System (INIS)

Yumaguzin, T.Kh.; Vyazovkin, D.E.; Nazirov, Eh.P.; Tuktarov, R.F.

1989-01-01

Synthesizer allows to set frequency with 0.015% accuracy and to scan it with variable step. Frequency controlled divider with further summing-up of divided frequency with fundamental one is used in synthesizer, and it has allowed to use digit of the input code and to obtain 3-4 MHz frequency range. Variation of operation flowsheet in the other frequency range is possible. K-155 and K-531 series microcircuits were used during development

Green–white electroluminescence and green photoluminescence of zinc complexes

Energy Technology Data Exchange (ETDEWEB)

Janghouri, Mohammad; Mohajerani, Ezeddin [Laser and Plasma Research Institute, Shahid Beheshti University, G.C., Tehran 1983963113 (Iran, Islamic Republic of); Amini, Mostafa M.; Najafi, Ezzatollah [Department of Chemistry, Shahid Beheshti University, G.C., Tehran 1983963113 (Iran, Islamic Republic of)

2014-10-15

A series of zinc complexes has been synthesized and utilized as fluorescent materials in organic light-emitting diodes (OLEDs). All prepared complexes were characterized by elemental analysis (CHN), UV–vis, FT-IR and {sup 1}H NMR spectroscopy. The energy levels of zinc complexes were determined by cyclic voltammetry measurements. Devices with fundamental structure of ITO/PVK:PBD (50 nm)/zinc complexes/BCP (5 nm)/Alq{sub 3} (25 nm)/Al (180 nm) were fabricated. A green electroluminescence was obtained from thin film complexes at 25 nm thickness. When thickness of the complex bis(2-methylquinolin-8-olato)-bis[(acetato)-(methanol)zinc(II)] (B) in thin film decreased from 25 nm to 20, 18, and 12 nm, a white electroluminescence obtained. The white emission which was composed of blue and green attributed to the PVK:PBD blend and thickness of complex, respectively. With 12 nm thickness of complex, a maximum luminance of 4530 cd/m{sup 2} at a current density 398.32 mA/cm{sup 2} with CIE coordinates of 0.22 and 0.36 at 20 V was achieved. - Highlights: • Several new zinc complexes have been synthesized and utilized as fluorescent materials in OLEDs. • Photoluminescence emission of zinc complexes showed a red shift in respect to PVK:PBD blend. • Green electroluminescence emission from zinc complexes was achieved. • White emission has been obtained for an OLED by changing thickness of the zinc complex.

Green–white electroluminescence and green photoluminescence of zinc complexes

International Nuclear Information System (INIS)

Janghouri, Mohammad; Mohajerani, Ezeddin; Amini, Mostafa M.; Najafi, Ezzatollah

2014-01-01

A series of zinc complexes has been synthesized and utilized as fluorescent materials in organic light-emitting diodes (OLEDs). All prepared complexes were characterized by elemental analysis (CHN), UV–vis, FT-IR and 1 H NMR spectroscopy. The energy levels of zinc complexes were determined by cyclic voltammetry measurements. Devices with fundamental structure of ITO/PVK:PBD (50 nm)/zinc complexes/BCP (5 nm)/Alq 3 (25 nm)/Al (180 nm) were fabricated. A green electroluminescence was obtained from thin film complexes at 25 nm thickness. When thickness of the complex bis(2-methylquinolin-8-olato)-bis[(acetato)-(methanol)zinc(II)] (B) in thin film decreased from 25 nm to 20, 18, and 12 nm, a white electroluminescence obtained. The white emission which was composed of blue and green attributed to the PVK:PBD blend and thickness of complex, respectively. With 12 nm thickness of complex, a maximum luminance of 4530 cd/m 2 at a current density 398.32 mA/cm 2 with CIE coordinates of 0.22 and 0.36 at 20 V was achieved. - Highlights: • Several new zinc complexes have been synthesized and utilized as fluorescent materials in OLEDs. • Photoluminescence emission of zinc complexes showed a red shift in respect to PVK:PBD blend. • Green electroluminescence emission from zinc complexes was achieved. • White emission has been obtained for an OLED by changing thickness of the zinc complex

Facile synthesis of RuII Schiff base complexes: spectral characterization and antimicrobial applications

International Nuclear Information System (INIS)

Arunachalam, S.; Padma Priya, N.; Shahul Meeran, H.

2014-01-01

Diamagnetic ruthenium (II) complexes of the type (RuCl (CO) (pyridine) (L)) (where L = monobasic tridentate Schiff base ligands) were synthesized by the reactions of Schiff bases derived from the reactions of o-aminobenzoic acid and Knovenegal condensate of β - ketoesters and appropriate ruthenium metal precursor (RuHCl (CO) (PPh 3 ) 2 (py)). Elemental analyses and spectral (FT-IR, UV-Vi s and 1 H, 31 P NMR) studies of all the new synthesized complexes suggest the presence of an octahedral environment around the Ru II ion. Cyclic voltammograms of all the complexes display oxidation and reduction potentials. Superoxide dismutase activity (SOD) of these complexes has also been examined. These complexes were also subjected to study their biocidal activity against Staphylococcus epidermidis, Escherichia coli, Botrytis cinerea and Aspergillus niger. (author)

Rhenium(V) complexes with sulfur-containing amino acids

International Nuclear Information System (INIS)

Gagieva, S.Ch.; Tautieva, M.A.; Tsaloev, A.T.; Galimov, Yu.B.; Gagieva, L.Ch.; Belyaeva, T.N.

2007-01-01

Rhenium(V) complexes with 2-amino-4-(methylthio)butanoic acid (methionine, Met) and 2-amino-3-sulfopropionic acid (cysteine, Cys) have been synthesized. Depending on the initial reagent ratio, the resulting complexes contain one or two ligand molecules. On heating the compounds with one amino acid molecule, two hydrogen halide molecules are removed at 128-132 deg C to form a molecular complex. The composition, structure, and thermal stability of the complexes have been studied by elemental analysis, conductometry, IR spectroscopy, NMR, and mass spectrometry [ru

PP32 and SET/TAF-Iβ proteins regulate the acetylation of newly synthesized histone H4.

Science.gov (United States)

Saavedra, Francisco; Rivera, Carlos; Rivas, Elizabeth; Merino, Paola; Garrido, Daniel; Hernández, Sergio; Forné, Ignasi; Vassias, Isabelle; Gurard-Levin, Zachary A; Alfaro, Iván E; Imhof, Axel; Almouzni, Geneviève; Loyola, Alejandra

2017-11-16

Newly synthesized histones H3 and H4 undergo a cascade of maturation steps to achieve proper folding and to establish post-translational modifications prior to chromatin deposition. Acetylation of H4 on lysines 5 and 12 by the HAT1 acetyltransferase is observed late in the histone maturation cascade. A key question is to understand how to establish and regulate the distinct timing of sequential modifications and their biological significance. Here, we perform proteomic analysis of the newly synthesized histone H4 complex at the earliest time point in the cascade. In addition to known binding partners Hsp90 and Hsp70, we also identify for the first time two subunits of the histone acetyltransferase inhibitor complex (INHAT): PP32 and SET/TAF-Iβ. We show that both proteins function to prevent HAT1-mediated H4 acetylation in vitro. When PP32 and SET/TAF-Iβ protein levels are down-regulated in vivo, we detect hyperacetylation on lysines 5 and 12 and other H4 lysine residues. Notably, aberrantly acetylated H4 is less stable and this reduces the interaction with Hsp90. As a consequence, PP32 and SET/TAF-Iβ depleted cells show an S-phase arrest. Our data demonstrate a novel function of PP32 and SET/TAF-Iβ and provide new insight into the mechanisms regulating acetylation of newly synthesized histone H4. © The Author(s) 2017. Published by Oxford University Press on behalf of Nucleic Acids Research.

Physico-Chemical and In-vitro Microbial Studies of Newly Synthesis Organometallic Complexes

Directory of Open Access Journals (Sweden)

Isam Hussain Al-Karkhi

2014-05-01

Full Text Available Drugs normally synthesized to use as medication to treat diseases like cancer and microbial infections, these synthesized drugs were interested more than naturally-derived drugs which have been shows low activity or not as efficient against diseases. A new ligand 3-methylbenzyl (2Z-2-[1-(pyridin-4-ylethylidene]hydrazine carbodithioate (PE3MBC and its Cd(II, Cu(II, Co(II and Zn(II metal complexes. The new ligand and metal complexes were characterized via various physico-chemical and spectroscopic techniques. Cd(II complex show more activity against microbes and against cancer cell line MCF-7, while other complexes does not shows activity like cadmium complex, all the complexes does not shows any activity against MDAMB-231 cell line. The fatal of the cancer and the microbes cell was due to inhibition of DNA synthesis which was probably due to chelating with metals complexes, or could be referred to lipophilicity, presence of hydrophobic moiety in the complex molecule, also could be due to steric effects and electronic effects.

Investigation into organic boron compounds complexing. 25. Triaryl borane complexes with benzimidazole

Energy Technology Data Exchange (ETDEWEB)

Belonovich, M I; Lapkin, I I; Morozova, T L; Okatysheva, L Yu; Rybakova, M N; Yuzhakova, G A [Permskij Gosudarstvennyj Univ. (USSR)

1984-02-01

Coordination of organic boron compounds with heterocyclic ligands is studied. Substances containing one molecule of ligand per one molecule of triarylborane are extracted when mixing ether solution of triarylborane and alcohol solution of benzimidazole. Based on IR spectra it is stated that coordination with boron is realized at the expense of pyridine nitrogen atom of imidazole cycle. Dipole momenta are determined for synthesized complexes using Debye method.

Single molecule magnet behaviour in robust dysprosium-biradical complexes.

Science.gov (United States)

Bernot, Kevin; Pointillart, Fabrice; Rosa, Patrick; Etienne, Mael; Sessoli, Roberta; Gatteschi, Dante

2010-09-21

A Dy-biradical complex was synthesized and characterized down to very low temperature. ac magnetic measurements reveal single molecule magnet behaviour visible without any application of dc field. The transition to the quantum tunneling regime is evidenced. Photophysical and EPR measurements provide evidence of the excellent stability of these complexes in solution.

Multiheteromacrocycles that complex metal ions. Third progress report, 1 May 1976--30 April 1977

International Nuclear Information System (INIS)

Cram, D.J.

1977-01-01

The overall objective of this research is to design, synthesize and evaluate cyclic and polycyclic host organic compounds for their abilities to complex and lipophilize guest metal ions, their complexes and clusters. Host organic compounds consist of strategically placed solvating, coordinating and ion-pairing sites tied together by covalent bonds through hydrocarbon units around cavities shaped to be occupied by guest metal ions, or metal ions plus their ligands. Specificity in complexation is sought by matching the following properties of host and guest: cavity and metal ion sizes; geometric arrangements of binding sites; numbers of binding sites; characters of binding sites; and valences. The specific compounds synthesized and their complexing and lipophilizing properties are summarized

Well-Defined Copper(I) Fluoroalkoxide Complexes for Trifluoroethoxylation of Aryl and Heteroaryl Bromides

KAUST Repository

Huang, Ronglu; Huang, Yangjie; Lin, Xiaoxi; Rong, Mingguang; Weng, Zhiqiang

2015-01-01

© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. Copper(I) fluoroalkoxide complexes bearing dinitrogen ligands were synthesized and the structure and reactivity of the complexes toward trifluoroethoxylation, pentafluoropropoxylation

A sol-gel method to synthesize indium tin oxide nanoparticles

Institute of Scientific and Technical Information of China (English)

Xiuhua Li; Xiujuan xu; Xin Yin; Chunzhong Li; Jianrong Zhang

2011-01-01

Transparent conductive indium tin oxide (ITO) nanoparticles were synthesized by a novel sol-gel method.Granulated indium and tin were dissolved in HNO3 and partially complexed with citric acid.A sol-gel process was induced when tertiary butyl alcohol was added dropwise to the above solution.ITO nanoparticles with an average crystallite size of 18.5 nm and surface area of 32.6 m2/g were obtained after the gel was heat-treated at 700 C.The ITO nanoparticles showed good sinterability,the starting sintering temperature decreased sharply to 900 C,and the 1400 C sintered pellet had a density of 98.1 ％ of theoretical density (TD).

Synthesizing Modular Invariants for Synchronous Code

Directory of Open Access Journals (Sweden)

Pierre-Loic Garoche

2014-12-01

Full Text Available In this paper, we explore different techniques to synthesize modular invariants for synchronous code encoded as Horn clauses. Modular invariants are a set of formulas that characterizes the validity of predicates. They are very useful for different aspects of analysis, synthesis, testing and program transformation. We describe two techniques to generate modular invariants for code written in the synchronous dataflow language Lustre. The first technique directly encodes the synchronous code in a modular fashion. While in the second technique, we synthesize modular invariants starting from a monolithic invariant. Both techniques, take advantage of analysis techniques based on property-directed reachability. We also describe a technique to minimize the synthesized invariants.

Chirality sensing with stereodynamic copper(I) complexes.

Science.gov (United States)

De Los Santos, Zeus A; Legaux, Nicholas M; Wolf, Christian

2017-11-01

Three Cu(I) complexes derived from stereodynamic diphosphine ligands were synthesized and used for chirality sensing. The coordination of diamines and amino acids to these complexes generates distinct circular dichroism signals. The chiroptical sensor response allows determination of the absolute configuration and the enantiomeric excess of the analyte at low concentrations. This method is operationally simple, fast, and attractive for high-throughput sensing applications. © 2017 Wiley Periodicals, Inc.

Thin films of molecular materials synthesized from fisher's carbene ferrocenyl: Film formation and electrical properties

Energy Technology Data Exchange (ETDEWEB)

Sanchez-Vergara, M.E. [Coordinacion de Ingenieria Mecatronica. Escuela de Ingenieria, Universidad Anahuac del Norte. Avenida Lomas de la Anahuac s/n, Col. Lomas Anahuac, 52786, Huixquilucan (Mexico)], E-mail: elena.sanchez@anahuac.mx; Ortiz, A. [Instituto de Investigaciones en Materiales. Universidad Nacional Autonoma de Mexico. A. P. 70-360, 04510, Mexico, DF (Mexico); Alvarez-Toledano, C.; Moreno, A. [Instituto de Quimica, Universidad Nacional Autonoma de Mexico. Circuito Exterior, Ciudad Universitaria, 04510, Mexico, DF (Mexico); Alvarez, J.R. [Instituto Tecnologico y de Estudios Superiores de Monterrey, Campus Ciudad de Mexico. Calle del Puente 222, Col. Ejidos de Huipulco, 14380, Mexico, DF (Mexico)

2008-07-31

The synthesis of materials from Fisher's carbene ferrocenyl of the elements chromium, molybdenum and tungsten was carried out. The Fisher's compounds that were synthesized included the following combinations of two different metallic atoms: iron with chromium, iron with molybdenum and iron with tungsten. The molecular solids' preparation was done in electro-synthesis cells with platinum electrodes. Thin films were prepared by vacuum thermal evaporation on quartz substrates and crystalline silicon wafers. Pellets and thin films from these compounds were characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, energy-dispersive spectroscopy, atomic force microscopy and ellipsometry. The powder and thin films synthesized from these materials show the same intra-molecular bonds shown by infrared spectroscopy results, suggesting that thermal evaporation does not alter these bonds in spite of the thin films being amorphous, in contrast with other bimetallic complexes where material decomposition occurs. The differences in the conductivity values of the prepared films are very small, so they may be attributed to the different metallic ions employed in each case. The tungsten complex exhibits a higher conductivity than the molybdenum and chromium complexes at room temperature. Electrical conductivity values found for thin films are higher than for pellets made of the same molecular materials.

Synthesis and characterization of pure and Li⁺ activated Alq₃ complexes for green and blue organic light emitting diodes and display devices.

Science.gov (United States)

Bhagat, S A; Borghate, S V; Kalyani, N Thejo; Dhoble, S J

2014-08-01

Pure and Li(+)-doped Alq3 complexes were synthesized by simple precipitation method at room temperature, maintaining the stoichiometric ratio. These complexes were characterized by X-ray diffraction, ultraviolet-visible absorption and Fourier transform infrared and photoluminescence (PL) spectra. X-ray diffraction analysis reveals the crystalline nature of the synthesized complexes, while Fourier transform infrared spectroscopy confirm the molecular structure, the completion of quinoline ring formation and presence of quinoline structure in the metal complex. Ultraviolet-visible and PL spectra revealed that Li(+) activated Alq3 complexes exhibit the highest intensity in comparison to pure Alq3 phosphor. Thus, Li(+) enhances PL emission intensity when doped into Alq3 phosphor. The excitation spectra lie in the range of 383-456 nm. All the synthesized complexes other than Liq give green emission, while Liq gives blue emission with enhanced intensity. Thus, he synthesized phosphors are the best suitable candidates for green- and blue-emitting organic light emitting diode, PL liquid-crystal display and solid-state lighting applications. Copyright © 2013 John Wiley & Sons, Ltd.

Highly Divergent Mitochondrial ATP Synthase Complexes in Tetrahymena thermophila

NARCIS (Netherlands)

Nina, Praveen Balabaskaran; Dudkina, Natalya V.; Kane, Lesley A.; van Eyk, Jennifer E.; Boekema, Egbert J.; Mather, Michael W.; Vaidya, Akhil B.; Eisen, Jonathan A.

The F-type ATP synthase complex is a rotary nano-motor driven by proton motive force to synthesize ATP. Its F(1) sector catalyzes ATP synthesis, whereas the F(o) sector conducts the protons and provides a stator for the rotary action of the complex. Components of both F(1) and F(o) sectors are

Synthesis, Spectroscopic Characterization, and Biological Activities of Metal Complexes of 4-((4-Chlorophenyldiazenyl-2-((p-tolyliminomethylphenol

Directory of Open Access Journals (Sweden)

C. Anitha

2013-01-01

Full Text Available Azo Schiff base complexes of VO(II, Mn(II, Co(II, Ni(II, Cu(II, and Zn(II have been synthesized from 4-((4-chlorophenyldiazenyl-2-((p-tolyliminomethylphenol (CDTMP. The nature of bonding and the structural features of the complexes have been deduced from elemental analysis, molar conductance, magnetic susceptibility measurements, IR, UV-Vis, 1H-NMR, EPR, mass, SEM, and fluorescence spectral studies. Spectroscopic and other analytical studies reveal square-planar geometry for copper, square-pyramidal geometry for oxovanadium, and octahedral geometry for other complexes. The EPR spectra of copper(II complex in DMSO at 300 K and 77 K were recorded, and its salient features are reported. Antimicrobial studies against several microorganisms indicate that the complexes are more potent bactericides and fungicides than the ligand. The electrochemical behavior of the copper(II complex was studied by cyclic voltammetry. All the synthesized compounds can serve as potential photoactive materials as indicated from their characteristic fluorescence properties. The second harmonic conversion efficiency of the synthesized azo Schiff base was found to be higher than that of urea and KDP (potassium dihydrogen phosphate. SEM image of copper(II complex implies the crystalline state and surface morphology of the complex.

Screening the DNA interaction ability and antimicrobial activity of a few novel bioactive complexes tethering N-((2-aminophenyl)(phenyl)methylene)-4-nitroaniline

Energy Technology Data Exchange (ETDEWEB)

Muniyandi, Vellaichamy; Raman, Natarajan, E-mail: ramchem1964@gmail.com

2016-11-01

Few novel transition metal complexes having N-((2-aminophenyl)(phenyl)methylene)-4-nitroaniline were synthesized and characterized by elemental analyses, IR, {sup 1}H and {sup 13}C NMR, electronic, EPR and mass spectra, conductivity and magnetic susceptibility measurements. All the metal complexes adopted square planar geometrical arrangements. The DNA-binding properties of the metal(II) complexes have been investigated by electronic absorption, fluorescence, CD spectra, cyclic voltammetry, differential pulse voltammogram and viscosity measurements. The results obtained indicate that these complexes bind to DNA via an intercalation binding mode. DNA cleavage activities indicate that the metal complexes exhibit greater activity than the ligand. The antimicrobial screening reveals that all the metal complexes exhibit better activity than the free ligand. - Highlights: • The newly synthesized mixed-ligand metal complexes act as persistent intercalators. • These mixed-ligand metal complexes display better chemical nuclease activity. • They exhibit potential antimicrobial activity. • Novel DNA targeting metal complexes are synthesized.

Ni(II) complexes of dithiophosphonic acids

Indian Academy of Sciences (India)

aDepartment of Chemistry, Science and Research Branch, Islamic Azad ... The compounds were characterized by 1H, 13C and 31P NMR, IR spectroscopy and elemental analysis. The ... design and synthesize Ni(II) complexes with new ..... Yield: 86%. ..... 28 65. 18. Greenwood D 1989 Antimicrobial chemotherapy (New.

Syntheses, X-ray structures, solid state high-field electron paramagnetic resonance, and density-functional theory investigations on chloro and aqua Mn(II) mononuclear complexes with amino-pyridine pentadentate ligands.

Science.gov (United States)

Hureau, Christelle; Groni, Sihem; Guillot, Régis; Blondin, Geneviève; Duboc, Carole; Anxolabéhère-Mallart, Elodie

2008-10-20

The two pentadentate amino-pyridine ligands L5(2) and L5(3) (L5(2) and L5(3) stand for the N-methyl-N,N',N'-tris(2-pyridylmethyl)ethane-1,2-diamine and the N-methyl-N,N',N'-tris(2-pyridylmethyl)propane-1,3-diamine, respectively) were used to synthesize four mononuclear Mn(II) complexes, namely [(L5(2))MnCl](PF6) (1(PF6)), [(L5(3))MnCl](PF6) (2(PF6)), [(L5(2))Mn(OH2)](BPh4)2 (3(BPh4)2), and [(L5(3))Mn(OH2)](BPh4)2 (4(BPh4)2). The X-ray diffraction studies revealed different configurations for the ligand L5(n) (n = 2, 3) depending on the sixth exogenous ligand and/or the counterion. Solid state high-field electron paramagnetic resonance spectra were recorded on complexes 1-4 as on previously described mononuclear Mn(II) systems with tetra- or hexadentate amino-pyridine ligands. Positive and negative axial zero-field splitting (ZFS) parameters D were determined whose absolute values ranged from 0.090 to 0.180 cm(-1). Density-functional theory calculations were performed unraveling that, in contrast with chloro systems, the spin-spin and spin-orbit coupling contributions to the D-parameter are comparable for mixed N,O-coordination sphere complexes.

Static inverter with synchronous output waveform synthesized by time-optimal-response feedback

Science.gov (United States)

Kernick, A.; Stechschulte, D. L.; Shireman, D. W.

1976-01-01

Time-optimal-response 'bang-bang' or 'bang-hang' technique, using four feedback control loops, synthesizes static-inverter sinusoidal output waveform by self-oscillatory but yet synchronous pulse-frequency-modulation (SPFM). A single modular power stage per phase of ac output entails the minimum of circuit complexity while providing by feedback synthesis individual phase voltage regulation, phase position control and inherent compensation simultaneously for line and load disturbances. Clipped sinewave performance is described under off-limit load or input voltage conditions. Also, approaches to high power levels, 3-phase arraying and parallel modular connection are given.

Equilibrium between Different Coordination Geometries in Oxidovanadium(IV) Complexes

Science.gov (United States)

Ugone, Valeria; Garribba, Eugenio; Micera, Giovanni; Sanna, Daniele

2015-01-01

In this laboratory activity, the equilibrium between square pyramidal and octahedral V(IV)O[superscript 2+] complexes is described. We propose a set of experiments to synthesize and characterize two types of V(IV)O[superscript 2+] complexes. The experiment allows great flexibility and may be effectively used at a variety of levels and the activity…

Studies on Oligomer Metal Complexes Derived from Bisamic Acid of Pyromellitic Dianhydride and 4-Bromoaniline.

Science.gov (United States)

Patel, Yogesh S

2014-01-01

Novel oligomer metal complexes (2a-f) of the ligand 2,5-bis((4-bromophenyl)carbamoyl) terephthalic acid (1) were prepared using transition metal salts and characterized by various spectroscopic techniques. The geometry of oligomer metal complexes was carried out by electronic spectral analysis and magnetic measurement studies. Polymeric properties have also been carried out. Ligand was synthesized using pyromellitic dianhydride and 4-bromoaniline. It was duly characterized. All novel synthesized compounds 1 and 2a-f were evaluated for their antibacterial and antifungal activity. The results showed significantly higher antibacterial and antifungal activity of oligomer metal complexes compared to the ligand.

Self-assembly of Terbium(III)-based metal-organic complexes with two-photon absorbing active

Science.gov (United States)

Li, Dandan; Shao, Nanqi; Sun, Xianshun; Zhang, Guocui; Li, Shengli; Zhou, Hongping; Wu, Jieying; Tian, Yupeng

2014-12-01

Hybrid complexes based on D-π-A type dyes p-aminostyryl-pyridinum and Terbium(III) complex anion (1, 2) have been synthesized by ionic exchange reaction. Meanwhile two different alkyl-substituted amino groups were used as electron donors in organic dyes cations. The synthesized complexes were characterized by element analysis. In addition, the structural features of them were systematic studied by single crystal X-ray diffraction analysis. Their linear properties have been systematically investigated by absorption spectra and fluorescence, the results show that the energy transfer takes place from the trans-4-[4‧-(N,N-diethylamino)styryl]-N-methyl pyridinium (2‧) cation to Tb(III). In addition, complex 2 exhibit a large two-photon absorption coefficient β: 0.044 cm/GW at 710 nm.

Isolated tumoral pyruvate dehydrogenase can synthesize acetoin which inhibits pyruvate oxidation as well as other aldehydes.

Science.gov (United States)

Baggetto, L G; Lehninger, A L

1987-05-29

Oxidation of 1 mM pyruvate by Ehrlich and AS30-D tumor mitochondria is inhibited by acetoin, an unusual and important metabolite of pyruvate utilization by cancer cells, by acetaldehyde, methylglyoxal and excess pyruvate. The respiratory inhibition is reversed by other substrates added to pyruvate and also by 0.5 mM ATP. Kinetic properties of pyruvate dehydrogenase complex isolated from these tumor mitochondria have been studied. This complex appears to be able to synthesize acetoin from acetaldehyde plus pyruvate and is competitively inhibited by acetoin. The role of a new regulatory pattern for tumoral pyruvate dehydrogenase is presented.

Antimalarial, antimicrobial, cytotoxic, DNA interaction and SOD like activities of tetrahedral copper(II) complexes

Science.gov (United States)

Mehta, Jugal V.; Gajera, Sanjay B.; Patel, Mohan N.

2015-02-01

The mononuclear copper(II) complexes with P, O-donor ligand and different fluoroquinolones have been synthesized and characterized by elemental analysis, electronic spectra, TGA, EPR, FT-IR and LC-MS spectroscopy. An antimicrobial efficiency of the complexes has been tested against five different microorganisms in terms of minimum inhibitory concentration (MIC) and displays very good antimicrobial activity. The binding strength and binding mode of the complexes with Herring Sperm DNA (HS DNA) have been investigated by absorption titration and viscosity measurement studies. The studies suggest the classical intercalative mode of DNA binding. Gel electrophoresis assay determines the ability of the complexes to cleave the supercoiled form of pUC19 DNA. Synthesized complexes have been tested for their SOD mimic activity using nonenzymatic NBT/NADH/PMS system and found to have good antioxidant activity. All the complexes show good cytotoxic and in vitro antimalarial activities.

Sorption of mercury on chemically synthesized polyaniline

International Nuclear Information System (INIS)

Remya Devi, P.S.; Verma, R.; Sudersanan, M.

2006-01-01

Sorption of inorganic mercury (Hg 2+ ) and methyl mercury, on chemically synthesized polyaniline, in 0.1-10N HCl solutions has been studied. Hg 2+ is strongly sorbed at low acidities and the extent of sorption decreases with increase in acidity. The sorption of methyl mercury is very low in the HCl concentration range studied. Sorption of Hg 2+ on polyaniline in 0.1-10N LiCl and H 2 SO 4 solutions has also been studied. The analysis of the data indicates that the sorption of Hg 2+ depends on the degree of protonation of polyaniline and the nature of mercury(II) chloride complexes in solution. X-ray photoelectron spectroscopy analysis (XPS) of polyaniline sorbed with mercury show that mercury is bound as Hg 2+ . Sorbed mercury is quantitatively eluted from polyaniline with 0.5N HNO 3 . Polyaniline can be used for separation and pre-concentration of inorganic mercury from aqueous samples. (author)

Reactivity of Fe3(CO)12 with Alkynes R-C≡-C-R':Syntheses and Crystal Structures of Substituted Cyclic Ketones and Carbonyl Iron Complexes

Institute of Scientific and Technical Information of China (English)

SUO Quan-Ling; WU Le; SU Qian; ZHU Ning; GAO Yuan-Yuan; HONG Hai-Long; XIE Rui-Jun; HAN Li-Min

2017-01-01

The reactivity of carbonyl iron cluster with alkynes has been studied by the thermal reaction of Fe3(CO)12 with R-C≡C-R'(R =Fc (Ferrocenyl);R'=Ph (Phenyl),Fc,H).The hexacarbonyldiiron cluster with ferracyclopentadiene ring (μ2,η4-C4Ph4)Fe2(CO)6 (1) and one tetraphenyl substituted cyclopentadienone (Ph4C4CO) (2) were simultaneously obtained by the reaction of Fe3(CO)12 with alkyne (Ph-C≡C-Ph).Only one ferrole cluster (μ2,η4-C4Fc2H2)Fe2(CO)6 (3) was separated by using Fc-C≡C-H as alkyne.One tri-carbonyl iron complex (η4-C4Fc4CO)Fe(CO)3 (4) and an unexpected new cyclic ketone compound 2,2,4,5-tetraferrocenylcyclopenta-4-en-l,3-di-one [Fc4C3(CO)2] (5) were obtained by using Fc-C≡C-Fc as alkyne.A new complex (η4-2,4-diphenyl-3,5-diferrocenylcyclopenta-2,4-dien-l-one)-tricarbonyl iron (η4-C4Ph2Fc2CO)Fe(CO)3 (6)was synthesized by the reaction of Fe3(CO)12 with Fc-C≡C-Ph.The structures of compounds 1～6 were determined by X-ray single-crystal diffraction and spectroscopic characterization.The crystal structures of two new compounds 5 and 6 were analyzed.Our experimental results reveal the structural models of the reaction products are affected by the kinds of substituents from alkynes R-C≡C-R'.

N-BUTYL SUBSTITUTED N-HETEROCYCLIC CARBENE-PD(II-PYRIDINE (PEPPSI COMPLEXES: SYNTHESIS, CHARACTERIZATION AND CATALYTIC ACTIVITY IN THE SUZUKI-MIYAURA REACTION

Directory of Open Access Journals (Sweden)

Rukiye Fırıncı

2016-08-01

Full Text Available A series of N-butyl substituted imidazolium salts, (1a-c and their pyridine enhanced precatalyst preparation stabilization and initiation (PEPPSI themed palladium N-heterocyclic carbene complexes (2a-c were synthesized and characterized. Pd-NHC complexes were fully determined by elemental analysis and spectroscopic. The synthesized complexes were tested in Suzuki-Miyaura cross-coupling reaction. These complexes were found to be efficient catalysts for the Suzuki-Miyaura reaction of phenylboronic acid with aryl bromides.

Assessment voice synthesizers for reading in digital books

Directory of Open Access Journals (Sweden)

Sérvulo Fernandes da Silva Neto

2013-07-01

Full Text Available The digital accessibility shows ways to information access in digital media that assist people with different types of disabilities to a better interaction with the computer independent of its limitations. Of these tools are composed by voice synthesizers, that supposedly simplifying their access to any recorded knowledge through digital technologies. However such tools have emerged originally in countries foreign language. Which brings us to the following research problem: the voice synthesizers are appropriate for reading digital books in the Portuguese language? The objective of this study was to analyze and classify different software tools voice synthesizers in combination with software digital book readers to support accessibility to e-books in Portuguese. Through literature review were identified applications software voice synthesizers, composing the sample analyzed in this work. We used a simplified version of the method of Multiple Criteria Decision Support - MMDA, to assess these. In the research 12 were considered readers of e-books and 11 software voice synthesizer, tested with six formats of e-books (E-pub, PDF, HTML, DOC, TXT, and Mobi. In accordance with the results, the software Virtual Vision achieved the highest score. Relative to formats, it was found that the PDF has measured a better score when summed the results of the three synthesizers. In the studied universe contacted that many synthesizers simply cannot be used because they did not support the Portuguese language.

The blue complexes of U in aqueous solutions

International Nuclear Information System (INIS)

Musikas, C.

1976-01-01

Mixed-valence uranium complexes were synthesized. Hydrolysis of hexavalent U leads to anionic species soluble in aqueous solutions when the UO 2 ++ ions are neutralized by tetraalkylammonium hydroxides. These complexes are polynuclear and the size and interatomic distances found for the polyanions are those of macromolecules. By hydrazine of these complexes, solutions were obtained and their absorption spectra studied. The spectra of U(VI) and U(V) ions are observed, together with new bands attributable to a charge transfer. It may be concluded that the blue complexes of uranium are type II composite-valence complexes for which the delocalization coefficient α can be calculated [fr

Synthesis and Spectral Characterization of Antifungal Sensitive Schiff Base Transition Metal Complexes

Science.gov (United States)

Sakthivel, A.; Rajasekaran, K.

2007-01-01

New N2O2 donor type Schiff base has been designed and synthesized by condensing acetoacetanilido-4-aminoantipyrine with 2-aminobenzoic acid in ethanol. Solid metal complexes of the Schiff base with Cu(II), Ni(II), Co(II), Mn(II), Zn(II), VO(IV), Hg(II) and Cd(II) metal ions were synthesized and characterized by elemental analyses, magnetic susceptibility, molar conduction, fast atom bombardment (FAB) mass, IR, UV-Vis, and 1H NMR spectral studies. The data show that the complexes have the composition of ML type. The UV-Vis. and magnetic susceptibility data of the complexes suggest a square-planar geometry around the central metal ion except VO(IV) complex which has square-pyramidal geometry. The in vitro antifungal activities of the compounds were tested against fungi such as Aspergillus niger, Aspergillus flavus, Rhizopus stolonifer, Candida albicans, Rhizoctonia bataicola and Trichoderma harizanum. All the metal complexes showed stronger antifungal activities than the free ligand. The minimum inhibitory concentrations (MIC) of the metal complexes were found in the range of 10~31 µg/ml. PMID:24015086

Perception of Paralinguistic Traits in Synthesized Voices

DEFF Research Database (Denmark)

Baird, Alice Emily; Hasse Jørgensen, Stina; Parada-Cabaleiro, Emilia

2017-01-01

Along with the rise of artificial intelligence and the internet-of-things, synthesized voices are now common in daily–life, providing us with guidance, assistance, and even companionship. From formant to concatenative synthesis, the synthesized voice continues to be defined by the same traits we...

Photocatalytic properties of hierarchical ZnO flowers synthesized by a sucrose-assisted hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Lv Wei [Key Laboratory of Photonic and Electric Bandgap Materials, Ministry of Education, School of Physics and Electronic Engineering, Harbin Normal University, Harbin 150025 (China); Wei Bo [Center for Condensed Matter Science and Technology, Department of Physics, Harbin Institute of Technology, Harbin 150080 (China); Xu Lingling, E-mail: xulingling_hit@163.com [Key Laboratory of Photonic and Electric Bandgap Materials, Ministry of Education, School of Physics and Electronic Engineering, Harbin Normal University, Harbin 150025 (China) and Center for Condensed Matter Science and Technology, Department of Physics, Harbin Institute of Technology, Harbin 150080 (China); Zhao Yan, E-mail: zhaoyan516@126.com [Department of Physics, Northeast Forestry University, Harbin 150040 (China); Gao Hong; Liu Jia [Key Laboratory of Photonic and Electric Bandgap Materials, Ministry of Education, School of Physics and Electronic Engineering, Harbin Normal University, Harbin 150025 (China)

2012-10-15

Highlights: Black-Right-Pointing-Pointer Hierarchical ZnO flowers were synthesized via a sucrose-assisted urea hydrothermal method. Black-Right-Pointing-Pointer The sucrose added ZnO flowers showed improved activity mainly due to the improved crystallinity. Black-Right-Pointing-Pointer The effect of sucrose content was studied and optimized. - Abstract: In this work, hierarchical ZnO flowers were synthesized via a sucrose-assisted urea hydrothermal method. The thermogravimetric analysis/differential thermal analysis (TGA-DTA) and Fourier transform infrared spectra (FTIR) showed that sucrose acted as a complexing agent in the synthesis process and assisted combustion during annealing. Photocatalytic activity was evaluated using the degradation of organic dye methyl orange. The sucrose added ZnO flowers showed improved activity, which was mainly attributed to the better crystallinity as confirmed by X-ray photoelectron spectroscopy (XPS) analysis. The effect of sucrose amount on photocatalytic activity was also studied.

3-Methylindole-Based Tripodal Tetraphosphine Ruthenium Complexes in N2 Coordination and Reduction and Formic Acid Dehydrogenation

Directory of Open Access Journals (Sweden)

Fenna F. van de Watering

2017-10-01

Full Text Available The ruthenium(II complexes RuCl2L1H, RuCl2L1CF3, RuCl2L1OMe and RuCl2L2H were synthesized from [Ru(η6-benzeneCl(μ-Cl]2 and the corresponding tripodal tris-3-methylindolephosphine-based ligands L1H, L1CF3, L1OMe, and L2H. Stoichiometric reduction of these complexes with KC8 yielded the corresponding ruthenium(0 dinitrogen complexes. The latter complexes were studied in the N2 reduction with chlorosilanes and KC8, yielding stoichiometric amounts of the silylamines. The synthesized ruthenium(II complexes are also active catalysts for the formic acid dehydrogenation reaction.

Particle size and shape modification of hydroxyapatite nanostructures synthesized via a complexing agent-assisted route

International Nuclear Information System (INIS)

Mohandes, Fatemeh; Salavati-Niasari, Masoud

2014-01-01

In this work, hydroxyapatite (HAP), Ca 10 (PO 4 ) 6 (OH) 2 , nanostructures including nanorods, nanobundles and nanoparticles have been prepared via a simple precipitation method. In the present method, Ca(NO 3 ) 2 ·4H 2 O and (NH 4 ) 2 HPO 4 were used as calcium and phosphorus precursors, respectively. Besides, the Schiff bases derived from 2-hydroxyacetophenone and different diamines were used as complexing agents for the in situ formation of Ca 2+ complexes. The formation mechanism of 0-D and 1-D nanostructures of HAP was also considered. When the complexing agents could coordinate to the Ca 2+ ions through N and O atoms to form the [CaN 2 O 2 ] 2+ complexes, HAP nanoparticles were generated. On the other hand, nanorods and nanobundles of HAP were obtained by forming the [CaN 2 ] 2+ as well as [CaO 2 ] 2+ complexes in the reaction solution. This work is the first successful synthesis of pure HAP nanostructures in the presence of Schiff bases instead of using the common surfactants. - Highlights: • HAP nanostructures have been prepared by a simple precipitation method. • To control shape and particle size of HAP, different Schiff bases were employed. • 0-D and 1-D HAP nanostructures have been formed by this method

Conceptualizing and measuring energy security: A synthesized approach

International Nuclear Information System (INIS)

Sovacool, Benjamin K.; Mukherjee, Ishani

2011-01-01

This article provides a synthesized, workable framework for analyzing national energy security policies and performance. Drawn from research interviews, survey results, a focused workshop, and an extensive literature review, this article proposes that energy security ought to be comprised of five dimensions related to availability, affordability, technology development, sustainability, and regulation. We then break these five dimensions down into 20 components related to security of supply and production, dependency, and diversification for availability; price stability, access and equity, decentralization, and low prices for affordability; innovation and research, safety and reliability, resilience, energy efficiency, and investment for technology development; land use, water, climate change, and air pollution for sustainability; and governance, trade, competition, and knowledge for sound regulation. Further still, our synthesis lists 320 simple indicators and 52 complex indicators that policymakers and scholars can use to analyze, measure, track, and compare national performance on energy security. The article concludes by offering implications for energy policy more broadly. -- Highlights: → Energy security should consist of five dimensions related to availability, affordability, technology development, sustainability, and regulation. → The dimensions of energy security can be broken down into 20 components. → These components can be distilled into 320 simple indicators and 52 complex indicators.

A fully integrated multi-standard frequency synthesizer for GNSS receivers with cellular network positioning capability

Science.gov (United States)

Bin, Li; Xiangning, Fan; Wei, Li; Li, Zhang; Zhigong, Wang

2013-01-01

A fully integrated hybrid integer/fractional frequency synthesizer is presented. With a single multiband voltage-controlled-oscillator (VCO), the frequency synthesizer can support GPS, Galileo, Compass and TD-SCDMA standards. Design is carefully performed to trade off power, die area and phase noise performance. By reconfiguring between the integer mode and fractional mode, different frequency resolution requirements and a constant loop bandwidth for each standard can be achieved simultaneously. Moreover, a long sequence length, reduced hardware complexity multi-stage-noise-shaping (MASH) Δ-Σ modulator is employed to reduce fractional spur in the fractional mode. Fabricated in a 0.18 μm CMOS technology, the frequency synthesizer occupies an active area of 1.48 mm2 and draws a current of 13.4-16.2 mA from a 1.8 V power supply. The measured phase noise is lower than -80 dBc/Hz at 100 kHz offset and -113 to -124 dBc/Hz at 1 MHz offset respectively, while the measured reference spur is -71 dBc in integer mode and the fractional spur is -65 dBc in fractional mode.

A fully integrated multi-standard frequency synthesizer for GNSS receivers with cellular network positioning capability

International Nuclear Information System (INIS)

Li Bin; Fan Xiangning; Li Wei; Zhang Li; Wang Zhigong

2013-01-01

A fully integrated hybrid integer/fractional frequency synthesizer is presented. With a single multiband voltage-controlled-oscillator (VCO), the frequency synthesizer can support GPS, Galileo, Compass and TD-SCDMA standards. Design is carefully performed to trade off power, die area and phase noise performance. By reconfiguring between the integer mode and fractional mode, different frequency resolution requirements and a constant loop bandwidth for each standard can be achieved simultaneously. Moreover, a long sequence length, reduced hardware complexity multi-stage-noise-shaping (MASH) Δ−Σ modulator is employed to reduce fractional spur in the fractional mode. Fabricated in a 0.18 μm CMOS technology, the frequency synthesizer occupies an active area of 1.48 mm 2 and draws a current of 13.4–16.2 mA from a 1.8 V power supply. The measured phase noise is lower than −80 dBc/Hz at 100 kHz offset and −113 to −124 dBc/Hz at 1 MHz offset respectively, while the measured reference spur is −71 dBc in integer mode and the fractional spur is −65 dBc in fractional mode. (semiconductor integrated circuits)

Raman assisted lightwave synthesized frequency sweeper

DEFF Research Database (Denmark)

Pedersen, Anders Tegtmeier; Rottwitt, Karsten

2010-01-01

We present a Lightwave Synthesized Frequency Sweeper comprising a Raman amplifier for loss compensation. The generated pulse train contains 123 pulses and has a flat signal level as well as a low noise level.......We present a Lightwave Synthesized Frequency Sweeper comprising a Raman amplifier for loss compensation. The generated pulse train contains 123 pulses and has a flat signal level as well as a low noise level....

Luminescent lanthanide coordination polymers

Energy Technology Data Exchange (ETDEWEB)

Ma, L.; Evans, O.R.; Foxman, B.M.; Lin, W.

1999-12-13

One-dimensional lanthanide coordination polymers with the formula Ln(isonicotinate){sub 3}(H{sub 2}O){sub 2} (Ln = Ce, Pr, Nd, Sm, Eu, Tb; 1a-f) were synthesized by treating nitrate or perchlorate salts of Ln(III) with 4-pyridinecarboxaldehyde under hydro(solvo)thermal conditions. Single-crystal and powder X-ray diffraction studies indicate that these lanthanide coordination polymers adopt two different structures. While Ce(III), Pr(III), and Nd(III) complexes adopt a chain structure with alternating Ln-(carboxylate){sub 2}-Ln and Ln-(carboxylate){sub 4}-Ln linkages, Sm(III), Eu(III), and Tb(III) complexes have a doubly carboxylate-bridged infinite-chain structure with one chelating carboxylate group on each metal center. In both structures, the lanthanide centers also bind to two water molecules to yield an eight-coordinate, square antiprismatic geometry. The pyridine nitrogen atoms of the isonicotinate groups do not coordinate to the metal centers in these lanthanide(III) complexes; instead, they direct the formation of Ln(III) coordination polymers via hydrogen bonding with coordinated water molecules. Photoluminescence measurements show that Tb(isonicotinate){sub 3}(H{sub 2}O){sub 2} is highly emissive at room temperature with a quantum yield of {approximately}90%. These results indicate that highly luminescent lanthanide coordination polymers can be assembled using a combination of coordination and hydrogen bonds. Crystal data for 1a: monoclinic space group P2{sub 1}/c, a = 9.712(2) {angstrom}, b = 19.833(4) {angstrom}, c = 11.616(2) {angstrom}, {beta} = 111.89(3){degree}, Z = 4. Crystal data for 1f: monoclinic space group C2/c, a = 20.253(4) {angstrom}, b = 11.584(2) {angstrom}, c = 9.839(2) {angstrom}, {beta} = 115.64(3){degree}, Z = 8.

Synthesis and characterization of hybrid silicon based complexing materials: extraction of transuranic elements from high level liquid waste; Synthese et caracterisation de gels hybrides de silice a proprietes complexantes: applications a l'extraction des transuraniens des effluents aqueux

Energy Technology Data Exchange (ETDEWEB)

Conocar, O

1999-07-01

Hybrid organic/inorganic silica compounds with extractive properties have been developed under an enhanced decontamination program for radioactive aqueous nitric acid waste in nuclear facilities. The materials were obtained by the sol-gel process through hydrolysis and poly-condensation of complexing organo-tri-alkoxy-silanes with the corresponding tetra-alkoxy-silane. Hybrid silica compounds were initially synthesized and characterized from mono- and bis-silyl precursors with malonamide or ethylenediamine patterns. Solids with different specific areas and pore diameters were obtained depending on the nature of the precursor, its functionality and its concentration in the tetra-alkoxy-silane. These compounds were then considered and assessed for use in plutonium and americium extraction. Excellent results-partitioning coefficients and capacities have been obtained with malonamide hybrid silica. The comparison with silica compounds impregnated or grafted with the same type of organic group is significant in this respect. Much of the improved performance obtained with hybrid silica may be attributed to the large quantity of complexing groups that can be incorporated in these materials. The effect of the solid texture on the extraction performance was also studied. Although the capacity increased with the specific area, little effect was observed on the distribution coefficients -notably for americium- indicating that the most favorable complexation sites are found on the outer surface. Macroporous malonamide hybrid silica compounds were synthesized to study the effects of the pore diameter, but the results have been inconclusive to date because of the unexpected molecular composition of the materials. (author)

Effect of zinc oxide nanoparticles synthesized by a precipitation

Indian Academy of Sciences (India)

ZnO nanoparticles were synthesized by a precipitation method in aqueous media from zinc nitrate hexahydrate and sodium hydroxide. The synthesized ZnO nanoparticles exhibited a crystalline structure with hexagonal structure of the wurtzite. The morphology of the synthesized ZnO nanoparticles presented a spherical ...

Group 4 Metalloporphyrin diolato Complexes and Catalytic Application of Metalloporphyrins and Related Transition Metal Complexes

Energy Technology Data Exchange (ETDEWEB)

Du, Guodong [Iowa State Univ., Ames, IA (United States)

2003-01-01

In this work, the first examples of group 4 metalloporphyrin 1,2-diolato complexes were synthesized through a number of strategies. In general, treatment of imido metalloporphyrin complexes, (TTP)M=NR, (M = Ti, Zr, Hf), with vicinal diols led to the formation of a series of diolato complexes. Alternatively, the chelating pinacolate complexes could be prepared by metathesis of (TTP)MCl₂ (M = Ti, Hf) with disodium pinacolate. These complexes were found to undergo C-C cleavage reactions to produce organic carbonyl compounds. For titanium porphyrins, treatment of a titanium(II) alkyne adduct, (TTP)Ti(η²-PhC≡CPh), with aromatic aldehydes or aryl ketones resulted in reductive coupling of the carbonyl groups to produce the corresponding diolato complexes. Aliphatic aldehydes or ketones were not reactive towards (TTP)Ti(η²-PhC≡CPh). However, these carbonyl compounds could be incorporated into a diolato complex on reaction with a reactive precursor, (TTP)Ti[O(Ph)₂C(Ph)₂O] to provide unsymmetrical diolato complexes via cross coupling reactions. In addition, an enediolato complex (TTP)Ti(OCPhCPhO) was obtained from the reaction of (TTP)Ti(η²-PhC≡CPh) with benzoin. Titanium porphyrin diolato complexes were found to be intermediates in the (TTP)Ti=O-catalyzed cleavage reactions of vicinal diols, in which atmospheric oxygen was the oxidant. Furthermore, (TTP)Ti=O was capable of catalyzing the oxidation of benzyl alcohol and α-hydroxy ketones to benzaldehyde and α-diketones, respectively. Other high valent metalloporphyrin complexes also can catalyze the oxidative diol cleavage and the benzyl alcohol oxidation reactions with dioxygen. A comparison of Ti(IV) and Sn(IV) porphyrin chemistry was undertaken. While chelated diolato complexes were invariably obtained for titanium porphyrins on treatment with 1,2-diols, the reaction of vicinal diols with tin porphyrins gave a number of products, including mono

Fluorido complexes of technetium

International Nuclear Information System (INIS)

Mariappan Balasekaran, Samundeeswari

2013-01-01

Fluorine chemistry has received considerable interest during recent years due to its significant role in the life sciences, especially for drug development. Despite the great nuclear medicinal importance of the radioactive metal technetium in radiopharmaceuticals, its coordination chemistry with the fluorido ligand is by far less explored than that of other ligands. Up to now, only a few technetium fluorides are known. This thesis contains the synthesis, spectroscopic and structural characterization of novel technetium fluorides in the oxidation states ''+1'', ''+2'', ''+4'' and ''+6''. In the oxidation state ''+6'', the fluoridotechnetates were synthesized either from nitridotechnetic(VI) acid or from pertechnetate by using reducing agent and have been isolated as cesium or tetraethylammonium salts. The compounds were characterized spectroscopically and structurally. In the intermediate oxidation state ''+4'', hexafluoridotechnetate(IV) was known for long time and studied spectroscopically. This thesis reports novel and improved syntheses and solved the critical issues of early publications such as the color, some spectroscopic properties and the structure of this key compound. Single crystal analyses of alkali metal, ammonium and tetramethylammonium salts of hexafluoridotechnetate(IV) are presented. In aqueous alkaline solutions, the ammonium salt of hexafluoridotechnetate(IV) undergoes hydrolysis and forms an oxido-bridged dimeric complex. It is the first step hydrolysis product of hexafluoridotechnetate(IV) and was characterized by spectroscopic and crystallographic methods. Low-valent technetium fluorides with the metal in the oxidation states of ''+2'' or ''+1'' are almost unknown. A detailed description of the synthesis and characterization of pentafluoridonitrosyltechnetate(II) is presented. The complex was isolated as alkali metal salts, and spectroscopic as well as structural features of the complexes are presented. Different salts of the trans

Synthesis, chemistry and catalytic activity of complexes of lanthanide and actinide metals in unusual oxidation states and coordination environments. Progress report, February 1, 1978--January 31, 1979

International Nuclear Information System (INIS)

Evans, W.J.

1978-11-01

Previous syntheses of Ln(olefin) complexes and their catalytic effect on the hydrogenation of the olefin are discussed. The tert-butyl complexes of Sn, Er, and Yb were synthesized and their decomposition studied

Charge-delocalized κ2 C, N-NHC-amine complexes of rhodium, iridium, and ruthenium

NARCIS (Netherlands)

Jansen, Eveline; Lutz, Martin; Bruin, Bas De; Elsevier, Cornelis J.

2014-01-01

The development of a novel set of complexes bearing an NHC-amine ligand (CNHC-NH2) is described. M(cod) complexes (M = Ir, Rh) and a Ru complex have been synthesized in which three different coordination modes of the ligand were established: monodentate, neutral bidentate, and anionic bidentate. The

Fe (III) complex of mefloquine hydrochloride: Synthesis ...

African Journals Online (AJOL)

As part of the ongoing research for more effective antimalarial drug, Fe (III) complex of mefloquine hydrochloride (antimalarial drug) was synthesized using template method. Mefloquine was tentatively found to have coordinated through the hydroxyl and the two nitrogen atoms in the quinoline and piperidine in the structure, ...

Nano magnetic solid phase extraction for preconcentration of lead ions in environmental samples by a newly synthesized reagent.

Science.gov (United States)

Golshekan, Mostafa; Shariati, Shahab

2013-01-01

In this study, magnetite nanoparticles with particle size lower than 47 nm were synthesized and were applied for preconcentration of Pb2+ ions from aqueous solutions. To preconcentrate the Pb2+ ions, the surface of the synthesized nano particles was modified with sodium dodecyl sulfate (SDS) as an anionic surfactant. A new chelating agent (2-((E)-2-amino-4,5-dinitrophenylimino)methyl)phenol) was synthesized and used to form a very stable complex with Pb2+ ions. The lead ions formed complexes and were quantitatively extracted with SDS-coated magnetite nanoparticles. After magnetic separation of adsorbent, the adsorbent was eluted with 0.5% (v/v) HC1 in dimethyl sulfoxide (DMSO) prior to analysis by flame atomic absorption spectrometry (FAAS). Orthogonal array design (OAD) was used to study and optimize the different experimental parameters. Under the optimum conditions, enhancement factor up to 63.5 was achieved for extraction from only 10 mL of sample solution and the relative standard deviation (RSD %) of the method was lower than 2.8%. The obtained calibration curve was linear in the range of 1-300 pg L-' with reasonable linearity (r2 > 0.998). The limit of detection (LOD) based on S/N = 3 was 0.04 microg L(-1) for 10 mL sample volumes. Finally, applicability of the proposed method was successfully confirmed by preconcentration and determination of trace amounts of lead ions in environmental samples and satisfactory results were obtained.

Synthesis, Characterization and Antibacterial Studies of N-(Benzothiazol-2-yl)-4-chlorobenzenesulphonamide and Its Neodymium(III) and Thallium(III) Complexes.

Science.gov (United States)

Obasi, Lawrence Nnamdi; Oruma, Uchechukwu Susan; Al-Swaidan, Ibrahim Abdulrazak; Ramasami, Ponnadurai; Ezeorah, Chigozie Julius; Ochonogor, Alfred Ezinna

2017-02-22

N -(Benzothiazol-2-yl)-4-chlorobenzenesulphonamide (NBTCS) was synthesized by condensation reaction of 4-chlorobenzenesulphonyl chloride and 2-aminobenzothiazole in acetone under reflux. Neodymium(III) and thallium(III) complexes of the ligand were also synthesized. Both ligand and metal complexes were characterized using UV-Vis, IR, ¹H- and 13 C-NMR spectroscopies, elemental analysis and molar conductance measurement. IR studies revealed that the ligand is tridentate and coordinates to the metal ions through nitrogen and oxygen atoms of the sulphonamide group and nitrogen atom attached to benzothiazole ring. The neodymium(III) complex displays a coordination number of eight while thallium(III) complex displays a coordination number of six. The ligand and its complexes were screened in vitro for their antibacterial activities against Escherichia coli strains ( E. coli 6 and E. coli 13 ), Proteus species, Staphylococcus aureus and Pseudomonas aeruginosa using the agar well diffusion technique. The synthesized compounds were found to be more active against the microorganisms screened relative to ciprofloxacin, gentamicin and co-trimoxazole.

Large-Scale Quantum Many-Body Perturbation on Spin and Charge Separation in the Excited States of the Synthesized Donor-Acceptor Hybrid PBI-Macrocycle Complex.

Science.gov (United States)

Ziaei, Vafa; Bredow, Thomas

2017-03-17

The reliable calculation of the excited states of charge-transfer (CT) compounds poses a major challenge to the ab initio community because the frequently employed method, time-dependent density functional theory (TD-DFT), massively relies on the underlying density functional, resulting in heavily Hartree-Fock (HF) exchange-dependent excited-state energies. By applying the highly sophisticated many-body perturbation approach, we address the encountered unreliabilities and inconsistencies of not optimally tuned (standard) TD-DFT regarding photo-excited CT phenomena, and present results concerning accurate vertical transition energies and the correct energetic ordering of the CT and the first visible singlet state of a recently synthesized thermodynamically stable large hybrid perylene bisimide-macrocycle complex. This is a large-scale application of the quantum many-body perturbation approach to a chemically relevant CT system, demonstrating the system-size independence of the quality of the many-body-based excitation energies. Furthermore, an optimal tuning of the ωB97X hybrid functional can well reproduce the many-body results, making TD-DFT a suitable choice but at the expense of introducing a range-separation parameter, which needs to be optimally tuned. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Well-defined mono(η3-allyl)nickel complex MONi(η3-C3H5) (M = Si or Al) grafted onto silica or alumina: A molecularly dispersed nickel precursor for syntheses of supported small size nickel nanoparticles

KAUST Repository

Li, Lidong; Abou-Hamad, Edy; Anjum, Dalaver H.; Zhou, Lu; Laveille, Paco; Emsley, Lyndon; Basset, Jean-Marie

2014-01-01

Preparing evenly-dispersed small size nickel nanoparticles over inert oxides remains a challenge today. In this context, a versatile method to prepare supported small size nickel nanoparticles (ca. 1-3 nm) with narrow size distribution via a surface organometallic chemistry (SOMC) route is described. The grafted mono(η3-allyl)nickel complexes MONi(η 3-C3H5) (M = Si or Al) as precursors are synthesized and fully characterized by elemental analysis, FTIR spectroscopy and paramagnetic solid-state NMR. © 2014 the Partner Organisations.

Experimental investigation of some coordination complexes using the sup(151)Eu Moessbauer resonance

International Nuclear Information System (INIS)

Lal, Asharfi; Rama Reddy, A.; Arvind; Ahmad, Naseer

1979-01-01

Several Schiff base complexes containing Eu 151 metal ions have been synthesized and their Moessbauer spectra are recorded using the constant acceleration velocity spectrometer. The least-square analysis method for the evaluation of the hyperfine field coupling constants is adopted using the computer dec system-10. From the systematic analysis of the quadrupole coupling constants (q.c.c.) and isomer shifts it has been established that the coordination number of the metal ion of Bis(acetylacetone) benzidine and thiourea complexes is five, that of bis-vanillin benzidine and bis-salicylaldehyde-o-dianisidine is six, and that of bis-vanillin-o-phenylene diamine is seven. It is also found that the q.c.c. being negative in all these complexes decreases monotonically as the coordination number increases. One unusual aspect of this experimental data is that most of the coordination complexes have very low f-factors whereas the Schiff base complexes studied here have a fairly high recoilless fractions. Attempts are in progress to synthesize and study the Fe Schiff base complexes in place of Eu. (auth.)

Charge-Delocalized κC-2,N-NHC-Amine Complexes of Rhodium, Iridium, and Ruthenium

NARCIS (Netherlands)

Jansen, E.; Lutz, M.; de Bruin, B.; Elsevier, C.J.

2014-01-01

The development of a novel set of complexes bearing an NHC-amine ligand (C-NHC-NH2) is described. M(cod) complexes (M = 1r, Rh) and a Ru complex have been synthesized in which three different coordination modes of the ligand were established: monodentate, neutral bidentate, and anionic bidentate.

Synthesis, crystal structures, and luminescent properties of two series' of new lanthanide (III) amino-carboxylate-phosphonates.

Science.gov (United States)

Zhou, Tian-Hua; Yi, Fei-Yan; Li, Pei-Xin; Mao, Jiang-Gao

2010-02-01

Hydrothermal reactions of lanthanide(III) chlorides with 4-HOOC-C(6)H(4)-CH(2)NHCH(2)PO(3)H(2) (H(3)L) at different ligand-to-metal (L/M) ratios afforded nine new lanthanide(III) carboxylate-phosphonates with two types of 3D network structures, namely, LnCl(HL)(H(2)O)(2) (Ln = Sm, 1; Eu, 2; Gd, 3; Tb, 4; Dy, 5; Er, 6) and [Ln(2)(HL)(H(2)L)(L)(H(2)O)(2)].4H(2)O (Ln = Nd, 7; Sm, 8; Eu, 9). Compounds 1-6 are isostructural and feature a 3D network in which the LnO(7)Cl polyhedra are interconnected by bridging CPO(3) tetrahedra into 2D inorganic layers parallel to the bc plane. These layers are further cross-linked by organic groups of the carboxylate-phosphonate ligands via the coordination of the carboxylate groups into a pillared-layered architecture. Compounds 7-9 are also isostructural and feature a 3D open-framework composed of 1D lanthanide(III) phosphonate inorganic slabs which are further bridged by organic groups of the carboxylate-phosphonate liagnds via the coordination of the carboxylate groups, forming large 1D tunnels along the b-axis which are filled by lattice water molecules. Luminescent measurements indicate that compounds 2, 4, and 5 show strong emission bands in red, green, and yellow light region, respectively. Magnetic properties of 2, 3, 5, and 7 have also been studied.

Affinity for a malignant tumor and organs of sup(99m)Tc-citrate complex

Energy Technology Data Exchange (ETDEWEB)

Ando, A; Sanada, S; Hiraki, T [Kanazawa Univ. (Japan). School of Paramedicine; Hisada, K; Nakazawa, N

1976-12-01

In order to investigate the tumor affinity of sup(99m)Tc-citrate complex, it was synthesized in three different ways. By (1) reducing sup(99m)TcO/sub 4//sup -/ with FeCl/sub 3//sup -/ ascorbic acid in 0.15 M sodium citrate, (2) reducing sup(99m)TcO/sub 4//sup -/ with SnCl/sub 2/ solution in 0.15 M sodium citrate, and (3) reducing sup(99m)TcO/sub 4//sup -/ with NaBH/sub 4/ in 0.45 sodium citrate. It was presumed from thinlayer chromatography that the sup(99m)Tc-citrate complexes synthesized in three ways were chemically different. These sup(99m)Tc-citrate complexes were injected intravenously into the rats subcutaneously transplanted with Yoshida sarcoma. These rats were sacrificed at one hour and three hours after injection. The radioactivity of the tumor, blood, muscle, liver, kidney, spleen and urine was measured by well-type scintillation counter. The retention values in these organs and the excretion rates in the urine were calculated. sup(99m)Tc-citrate complex synthesized by reducing sup(99m)TcO/sub 4//sup -/ with SnCl/sub 2/ solution had very strong affinity for the malignant tumor but the other two sup(99m)Tc-citrate complexes had no affinity to the malignant tumor. Excretion rates (% dose) of sup(99m)Tc-citrate complexes in one hour were from 65% to 75%.

Luminescent lanthanide coordination polymers synthesized via in-situ hydrolysis of dimethyl-3,4-furandicarboxylate

International Nuclear Information System (INIS)

Greig, Natalie E.; Einkauf, Jeffrey D.; Clark, Jessica M.; Corcoran, Eric J.; Karram, Joseph P.; Kent, Charles A.; Eugene, Vadine E.; Chan, Benny C.; Lill, Daniel T. de

2015-01-01

Dimethyl-3,4-furandicarboxylate undergoes hydrolysis under hydrothermal conditions with lanthanide (Ln) ions to form two-dimensional coordination polymers, [Ln(C 6 H 2 O 5 )(C 6 H 3 O 5 )(H 2 O)] n (Ln=Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu). The resulting materials exhibit luminescent properties with quantum yields and lifetimes for the Eu(III) and Tb(III) compounds of 1.1±0.3% and 0.387±0.0001 ms, and 3.3±0.8% and 0.769±0.006 ms, respectively. Energy values for the singlet and triplet states were determined for dimethyl-3,4-furandicarboxylate and 3,4-furandicarboxylic acid. Excited state dynamics and structural features are examined to explicate the reported quantum yields. A series of other FDC structures is briefly presented. - Graphical abstract: A new two-dimensional coordination polymer derived from the in-situ hydrolysis of a furan dimethyl ester with lanthanide(III) ions was obtained in order to study its photophysical behavior when constructed from trivalent Eu and Tb. Quantum yields, lifetime measurements, and singlet/triplet state energies values were obtained. The nature of the material's excited state dynamics is examined and correlated to its structure in order to explain the overall luminescent efficiency of the system. - Highlights: • A new lanthanide–furandicarboxylate coordination polymer is presented. • Eu and Tb compounds display luminescent properties, albeit with low quantum yields. • Photophysical behavior explained through the compound's triplet state and structure. • Nonradiative deactivation of luminescence through high-energy oscillators was noted. • Molecular modeling of the organic moiety was conducted

Luminescent lanthanide coordination polymers synthesized via in-situ hydrolysis of dimethyl-3,4-furandicarboxylate

Energy Technology Data Exchange (ETDEWEB)

Greig, Natalie E.; Einkauf, Jeffrey D.; Clark, Jessica M.; Corcoran, Eric J.; Karram, Joseph P.; Kent, Charles A.; Eugene, Vadine E. [Department of Chemistry & Biochemistry, Florida Atlantic University, 777 Glades Road, Boca Raton, FL 33431 (United States); Chan, Benny C. [Department of Chemistry, The College of New Jersey, 2000 Pennington Road, Ewing, NJ 08628 (United States); Lill, Daniel T. de, E-mail: ddelill@fau.edu [Department of Chemistry & Biochemistry, Florida Atlantic University, 777 Glades Road, Boca Raton, FL 33431 (United States)

2015-05-15

Dimethyl-3,4-furandicarboxylate undergoes hydrolysis under hydrothermal conditions with lanthanide (Ln) ions to form two-dimensional coordination polymers, [Ln(C{sub 6}H{sub 2}O{sub 5})(C{sub 6}H{sub 3}O{sub 5})(H{sub 2}O)]{sub n} (Ln=Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu). The resulting materials exhibit luminescent properties with quantum yields and lifetimes for the Eu(III) and Tb(III) compounds of 1.1±0.3% and 0.387±0.0001 ms, and 3.3±0.8% and 0.769±0.006 ms, respectively. Energy values for the singlet and triplet states were determined for dimethyl-3,4-furandicarboxylate and 3,4-furandicarboxylic acid. Excited state dynamics and structural features are examined to explicate the reported quantum yields. A series of other FDC structures is briefly presented. - Graphical abstract: A new two-dimensional coordination polymer derived from the in-situ hydrolysis of a furan dimethyl ester with lanthanide(III) ions was obtained in order to study its photophysical behavior when constructed from trivalent Eu and Tb. Quantum yields, lifetime measurements, and singlet/triplet state energies values were obtained. The nature of the material's excited state dynamics is examined and correlated to its structure in order to explain the overall luminescent efficiency of the system. - Highlights: • A new lanthanide–furandicarboxylate coordination polymer is presented. • Eu and Tb compounds display luminescent properties, albeit with low quantum yields. • Photophysical behavior explained through the compound's triplet state and structure. • Nonradiative deactivation of luminescence through high-energy oscillators was noted. • Molecular modeling of the organic moiety was conducted.

Copolymers containing phosphorescent iridium(III) complexes obtained by free and controlled radical polymerization techniques

NARCIS (Netherlands)

Ulbricht, C.; Becer, C.R.; Winter, A.; Veldman, D.; Schubert, U.S.

2008-01-01

A methacrylate-functionalized phosphorescent Ir(III)-complex has been synthesized, characterized, and applied as a monomer in radical copolymerizations. Together with methyl methacrylate, the complex has been copolymerized under free radical polymerization conditions. Aiming for host-guest-systems,

Preparation and Characterization of Double Metal Cyanide Complex Catalysts

Directory of Open Access Journals (Sweden)

Weilin Guo

2003-01-01

Full Text Available A series of double metal cyanide (DMC complex catalysts were prepared in two different methods by using ß-cyclodextrin, PEG-1000 and Tween-60 as an additional complex ligands respectively. It was showed that a mixture of crystalline and amorphous DMC was synthesized by using traditional method in which the additional complex ligand was added after the precipitation of DMC. Amorphous and dispersed DMC with higher activity could be obtained when the additional complex ligand was added in the reactant solution before reaction. The effect of additional complex ligand and preparation method on the crystalline state and catalytic property of DMC were also investigated.

Synthesis, spectral, thermal, potentiometric and antimicrobial studies of transition metal complexes of tridentate ligand

Directory of Open Access Journals (Sweden)

Sarika M. Jadhav

2014-01-01

Full Text Available A series of metal complexes of Cu(II, Ni(II, Co(II, Fe(III and Mn(II have been synthesized with newly synthesized biologically active tridentate ligand. The ligand was synthesized by condensation of dehydroacetic acid (3-acetyl-6-methyl-(2H pyran-2,4(3H-dione or DHA, o-phenylene diamine and fluoro benzaldehyde and characterized by elemental analysis, molar conductivity, magnetic susceptibility, thermal analysis, X-ray diffraction, IR, 1H-NMR, UV–Vis spectroscopy and mass spectra. From the analytical data, the stoichiometry of the complexes was found to be 1:2 (metal:ligand with octahedral geometry. The molar conductance values suggest the non-electrolyte nature of metal complexes. The IR spectral data suggest that the ligand behaves as a dibasic tridentate ligand with ONN donor atoms sequence towards central metal ion. Thermal behaviour (TG/DTA and kinetic parameters calculated by the Coats–Redfern and Horowitz–Metzger method suggest more ordered activated state in complex formation. To investigate the relationship between stability constants of metal complexes and antimicrobial activity, the dissociation constants of Schiff bases and stability constants of their binary metal complexes have been determined potentiometrically in THF–water (60:40% solution at 25 ± 1 °C and at 0.1 M NaClO4 ionic strength. The potentiometric study suggests 1:1 and 1:2 complexation. Antibacterial and antifungal activities in vitro were performed against Staphylococcus aureus, Escherichia coli and Aspergillus niger, Trichoderma, respectively. The stability constants of the metal complexes were calculated by the Irving–Rosotti method. A relation between the stability constant and antimicrobial activity of complexes has been discussed. It is observed that the activity enhances upon complexation and the order of antifungal activity is in accordance with stability order of metal ions.

Gd-Complexes of New Arylpiperazinyl Conjugates of DTPA-Bis(amides: Synthesis, Characterization and Magnetic Relaxation Properties

Directory of Open Access Journals (Sweden)

Abdullah O. Ba-Salem

2015-04-01

Full Text Available Two new DTPA-bis(amide based ligands conjugated with the arylpiperazinyl moiety were synthesized and subsequently transformed into their corresponding Gd(III complexes 1 and 2 of the type [Gd(LH2O]·nH2O. The relaxivity (R1 of these complexes was measured, which turned out to be comparable with that of Omniscan®, a commercially available MRI contrast agent. The cytotoxicity studies of these complexes indicated that they are non-toxic, which reveals their potential and physiological suitability as MRI contrast agents. All the synthesized ligands and complexes were characterized with the aid of analytical and spectroscopic methods, including elemental analysis, 1H-NMR, FT-IR, XPS and fast atom bombardment (FAB mass spectrometry.

Biological Screening of Newly Synthesized BIAN N-Heterocyclic Gold Carbene Complexes in Zebrafish Embryos

Science.gov (United States)

Farooq, Muhammad; Abu Taha, Nael; Butorac, Rachel R.; Evans, Daniel Anthony; Elzatahry, Ahmed A.; Elsayed, Elsayed Ahmed; Wadaan, Mohammad A. M.; Al-Deyab, Salem S.; Cowley, Alan H.

2015-01-01

N-Heterocyclic carbene (NHC) metal complexes possess diverse biological activities but have yet to be extensively explored as potential chemotherapeutic agents. We have previously reported the synthesis of a new class of NHC metal complexes N-heterocyclic with acetate [IPr(BIAN)AuOAc] and chloride [IPr(BIAN)AuCl] ligands. In the experiments reported herein, the zebrafish embryos were exposed to serial dilutions of each of these complexes for 10–12 h. One hundred percent mortality was observed at concentrations ≥50 µM. At sub-lethal concentrations (10–30 µM), both compounds influenced zebrafish embryonic development. However, quite diverse categories of abnormalities were found in exposed embryos with each compound. Severe brain deformation and notochord degeneration were evident in the case of [IPr(BIAN)AuOAc]. The zebrafish embryos treated with [IPr(BIAN)AuCl] exhibited stunted growth and consequently had smaller body sizes. A depletion of 30%–40% glutathione was detected in the treated embryos, which could account for one of the possible mechanism of neurotoxicity. The fact that these compounds are capable of both affecting the growth and also compromising antioxidant systems by elevating intracellular ROS production implies that they could play an important role as a new breed of therapeutic molecules. PMID:26501273

Controlled synthesized natroalunite microtubes applied for cadmium(II) and phosphate co–removal

Energy Technology Data Exchange (ETDEWEB)

Xu, Huan [School of Physics and Materials Science, Anhui University, Hefei 230601 (China); Institute of Plasma Physics, Chinese Academy of Sciences, P.O. Box 1126, Hefei 230031 (China); Zhu, Baisheng [University of Science and Technology of China, Hefei 230026 (China); Ren, Xuemei, E-mail: renxm1985@163.com [Institute of Plasma Physics, Chinese Academy of Sciences, P.O. Box 1126, Hefei 230031 (China); Shao, Dadong; Tan, Xiaoli; Chen, Changlun [Institute of Plasma Physics, Chinese Academy of Sciences, P.O. Box 1126, Hefei 230031 (China)

2016-08-15

Highlights: • Five natroalunite samples with different morphologies were synthesized. • EG: water ratio controls the morphology and adsorption performance of natroalunite. • NMs show the best performance in Cd(II) and phosphate co-uptake. • Phosphate bridges NMs and Cd(II) in co–removal process and enhances Cd(II) uptake. - Abstract: Treatment of wastewater containing several kinds of contaminants poses great challenges, because heavy metal and inorganic anion contaminants possess different fate and transport mechanisms. Individual adsorption of Cd(II)/phosphate on clay or metallic oxides has been extensively investigated, but the mutual effects of these two species in co–existing systems have received little attention. In this study, five natroalunite samples with different morphologies were synthesized by a simple hydrothermal method with appropriate volume ratio of ethylene glycol (EG) to water. The volume ratio of EG to water plays a key role in the formation of natroalunite samples, and dramatically affects their adsorption capacities. The mutual effects of Cd(II) and phosphate on their interaction with natroalunite microtubes (NMs) were investigated by varying experimental conditions, such as pH, temperature and addition sequences. The results demonstrate that highly efficient co–removal of Cd(II) and phosphate can be accomplished using NMs, and the process is strongly dependent on solution pH and temperature via the formation of ternary surface complexes. This study implies that the hydrothermally synthesized NMs can be regarded as a potential promising material for the co–removal of Cd(II) and phosphate from large volumes of aqueous solutions in pollution management.

Enantioselective catalytic syntheses of alpha-branched chiral amines

DEFF Research Database (Denmark)

Brase, S.; Baumann, T.; Dahmen, S.

2007-01-01

Chiral amines play a pivotal role in fine chemical and natural product syntheses and the design of novel materials.......Chiral amines play a pivotal role in fine chemical and natural product syntheses and the design of novel materials....

Nanoparticles of novel organotin(IV) complexes bearing phosphoric triamide ligands

Science.gov (United States)

Asadi, Ebadullah; Tavasolinasab, Vahid; Gholivand, Khodayar

2013-01-01

Summary Four novel organotin(IV) complexes containing phosphoric triamide ligands were synthesized and characterized by multinuclear (1H, 31P, 13C) NMR, infrared, ultraviolet and fluorescence spectroscopy as well as elemental analysis. The 1H NMR spectra of complexes 1–4 proved that the Sn atoms adopt octahedral configurations. The nanoparticles of the complexes were also prepared by ultrasonication, and their SEM micrographs indicated identical spherical morphologies with particles sizes about 20–25 nm. The fluorescence spectra exhibited blue shifts for the maximum wavelength of emission upon complexation. PMID:23504649

Structure and composition of iron nanoparticles synthesized using a novel anionic-element complex

Energy Technology Data Exchange (ETDEWEB)

Skoropata, E.; Desautels, R. D.; Lierop, J. van, E-mail: johan@physics.umanitoba.ca [Department of Physics and Astronomy, University of Manitoba, Winnipeg, Manitoba R3T 2N2 (Canada); Rowe, M. [Toyota Research Institute of North America, 1555 Woodridge Ave., Ann Arbor, Michigan 48105 (United States)

2015-05-07

We use a novel solution-based disassociation synthesis scheme of the ionic complex Fe(LiBH{sub 4}){sub 2} to form Fe nanoparticles. The complex was formed initially using a gentle mechanochemical process, and the Fe nanoparticles emerged after 4 h of ball milling in an air-free environment. Rietveld refinement of x-ray diffraction measurements in an air-free sample holder identified a Im3{sup ¯}m α-Fe phase. A room temperature Mössbauer spectrum of the sample presented a six-line spectrum unique to Fe{sup 0} metal, and the Fe nanoparticles were extremely well crystallized. Magnetometry results presented a reduced saturation magnetization (e.g., M{sub s}∼ 85 emu/g at 50 K) that had a Bloch-like T{sup 2} temperature dependence, consistent with a gap in the magnon fluctuation spectrum due to finite-size effects. The Fe nanoparticles were magnetically soft, with a coercivity ranging from ∼10 to 20 mT with decreasing temperature from 350 K.

The development of [18F]FDG synthesizer

International Nuclear Information System (INIS)

Hu, M. G.; Kim, S. W.; Lee, J. Y.; Yang, S. D.; Jun, G. S.

2003-01-01

The automatic system for [ 18 F]FDG production using for the diagnosis of cancer has been developed. This automation system was consisted of a synthesizer module, a PLC based controller and a PMU for graphic user interface. By this system, the radiochemical purity was over 98%, the production yield was over 30% after synthesize and elapsed time was 35 minute

Stabilization and augmentation of circulating AIM in mice by synthesized IgM-Fc.

Directory of Open Access Journals (Sweden)

Toshihiro Kai

Full Text Available Owing to rapid and drastic changes in lifestyle and eating habits in modern society, obesity and obesity-associated diseases are among the most important public health problems. Hence, the development of therapeutic approaches to regulate obesity is strongly desired. In view of previous work showing that apoptosis inhibitor of macrophage (AIM blocks lipid storage in adipocytes, thereby preventing obesity caused by a high-fat diet, we here explored a strategy to augment circulating AIM levels. We synthesized the Fc portion of the soluble human immunoglobulin (IgM heavy chain and found that it formed a pentamer containing IgJ as natural IgM does, and effectively associated with AIM in vitro. When we injected the synthesized Fc intravenously into mice lacking circulating IgM, it associated with endogenous mouse AIM, protecting AIM from renal excretion and preserving the circulating AIM levels. As the synthesized Fc lacked the antigen-recognizing variable region, it provoked no undesired immune response. In addition, a challenge with the Fc-human AIM complex in wild-type mice, which exhibited normal levels of circulating IgM and AIM, successfully maintained the levels of the human AIM in mouse blood. We also observed that the human AIM was effectively incorporated into adipocytes in visceral fat tissue, suggesting its functionality against obesity. Thus, our findings reveal potent strategies to safely increase AIM levels, which could form the basis for developing novel therapies for obesity.

Synthesis and characterization of chiral thorium(IV) and uranium(IV) benzamidinate complexes

Energy Technology Data Exchange (ETDEWEB)

Schoene, Sebastian; Maerz, Juliane; Kaden, Peter; Patzschke, Michael; Ikeda-Ohno, Atsushi [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Chemistry of the F-Elements

2017-06-01

Two chiral benzamidinate complexes of tetravalent actinides (Th(IV) and U(IV)) were synthesized using a salt metathesis reaction of the corresponding actinide(IV) tetrachlorides and the potassium salt of the chiral benzamidine (S,S)-N,N-Bis-(1-phenylethyl)-benzamidine ((S)-HPEBA). The structure of the complexes was determined with single crystal X-ray diffraction. These are the first examples of chiral amidinate complexes of actinides.

Syntheses and catalytic oxotransfer activities of oxo molybdenum(vi) complexes of a new aminoalcohol phenolate ligand.

Science.gov (United States)

Hossain, M K; Haukka, M; Sillanpää, R; Hrovat, D A; Richmond, M G; Nordlander, E; Lehtonen, A

2017-05-30

The new aminoalcohol phenol 2,4-di-tert-butyl-6-(((2-hydroxy-2-phenylethyl)amino)methyl)phenol (H2L) was prepared by a facile solvent-free synthesis and used as a tridentate ligand for new cis-dioxomolybdenum(vi)(L) complexes. In the presence of a coordinating solvent (DMSO, MeOH, pyridine), the complexes crystallise as monomeric solvent adducts while in the absence of such molecules, a trimer with asymmetric Mo[double bond, length as m-dash]O→Mo bridges crystallises. The complexes can catalyse epoxidation of cis-cyclooctene and sulfoxidation of methyl-p-tolylsulfide, using tert-butyl hydroperoxide as oxidant.

Syntheses and absorption-structure relationships of some new ...

Indian Academy of Sciences (India)

New biheterocyclic compound was synthesized as starting material to prepare new photosensitizers mono-, tri-, substituted tri-, azadimethine and mixed cyanine dyes. Absorption-structure relationship of the synthesized cyanine dyes were determined by studying their electronic spectral behaviour in ethanol. The structure of ...

Investigation of the complex structure, comparative DNA-binding and DNA cleavage of two water-soluble mono-nuclear lanthanum(III) complexes and cytotoxic activity of chitosan-coated magnetic nanoparticles as drug delivery for the complexes

Science.gov (United States)

Asadi, Zahra; Nasrollahi, Neda; Karbalaei-Heidari, Hamidreza; Eigner, Vaclav; Dusek, Michal; Mobaraki, Nabiallah; Pournejati, Roya

2017-05-01

Two water-soluble mono-nuclear macrocyclic lanthanum(III) complexes of 2,6-diformyl-4-methylphenol with 1,3-diamino-2-propanol (C1) or 1,3-propylenediamine (C2) were synthesized and characterized by UV-Vis, FT-IR, 13C and 1H NMR spectroscopy and elemental analysis. C1 complex was structurally characterized by single-crystal X-ray diffraction, which revealed that the complex was mononuclear and ten-coordinated. The coordination sites around lanthanum(III) were occupied with a five-dentate ligand, two bidentate nitrates, and one water molecule. The interaction of complexes with DNA was studied in buffered aqueous solution at pH 7.4. UV-Vis absorption spectroscopy, emission spectroscopy, circular dichroism (CD) and viscometric measurements provided clear evidence of the intercalation mechanism of binding. The obtained intrinsic binding constants (Kb) 9.3 × 103 and 1.2 × 103 M- 1 for C1 and C2, respectively confirmed that C1 is better intercalator than C2. The DNA docking studies suggested that the complexes bind with DNA in a groove binding mode with the binding affinity of C1 > C2. Moreover, agarose gel electrophoresis study of the DNA-complex for both compounds revealed that the C1 intercalation cause ethidium bromide replacement in a competitive manner which confirms the suggested mechanism of binding. Finally, the anticancer experiments for the treated cancerous cell lines with both synthesized compounds show that these hydrophilic molecules need a suitable carrier to pass through the hydrophobic nature of cell membrane efficiently.

Chiral PEPPSI Complexes: Synthesis, Characterization, and Application in Asymmetric Suzuki–Miyaura Coupling Reactions

KAUST Repository

Benhamou, Laure

2014-01-13

PEPPSI complexes incorporating chiral N-heterocyclic carbene (NHC) ligands based on 2,2-dimethyl-1-(o-substituted aryl)propan-1-amines were synthesized. Two complexes, with one saturated and one unsaturated NHC ligand, were structurally characterized. The chiral PEPPSI complexes were used in asymmetric Suzuki-Miyaura reactions, giving atropisomeric biaryl products in modest to good enantiomeric ratios. © 2013 American Chemical Society.

Chiral PEPPSI Complexes: Synthesis, Characterization, and Application in Asymmetric Suzuki–Miyaura Coupling Reactions

KAUST Repository

Benhamou, Laure; Besnard, Cé line; Kü ndig, E. Peter

2014-01-01

PEPPSI complexes incorporating chiral N-heterocyclic carbene (NHC) ligands based on 2,2-dimethyl-1-(o-substituted aryl)propan-1-amines were synthesized. Two complexes, with one saturated and one unsaturated NHC ligand, were structurally characterized. The chiral PEPPSI complexes were used in asymmetric Suzuki-Miyaura reactions, giving atropisomeric biaryl products in modest to good enantiomeric ratios. © 2013 American Chemical Society.

Structural characterization and antimicrobial activities of transition metal complexes of a hydrazone ligand

Science.gov (United States)

Bakale, Raghavendra P.; Naik, Ganesh N.; Machakanur, Shrinath S.; Mangannavar, Chandrashekhar V.; Muchchandi, Iranna S.; Gudasi, Kalagouda B.

2018-02-01

A hydrazone ligand has been synthesized by the condensation of 2-nitrobenzaldehyde and hydralazine, and its Co(II), Ni(II), Cu(II) and Zn(II) complexes have been reported. Structural characterization of the ligand and its metal complexes has been performed by various spectroscopic [IR, NMR, UV-Vis, Mass], thermal and other physicochemical methods. The structure of the ligand and its Ni(II) complex has been characterized by single crystal X-ray diffraction studies. All the synthesized compounds have been screened for in vitro antimicrobial activity. The antibacterial activity is tested against Gram-positive strains Enterococcus faecalis, Streptococcus mutans and Staphylococcus aureus and Gram-negative strains Escherichia coli, Pseudomonas aeruginosa and Klebsiella pneumoniae using ciprofloxacin as the reference standard. Antifungal activity is tested against Candida albicans, Aspergillus fumigatus and Aspergillus niger using ketoconazole as the reference standard. The minimum inhibitory concentration (MIC) was determined for test compounds as well as for reference standard. Ligand, Cu(II) and Zn(II) complexes have shown excellent activity against Candida albicans.

Lewis base binding affinities and redox properties of plutonium complexes

International Nuclear Information System (INIS)

Oldham, Susan M.; Schake, Ann R.; Burns, Carol J.; Morgan, Arthur N. III; Schnabel, Richard C.; Warner, Benjamin P.; Costa, David A.; Smith, Wayne H.

2000-01-01

As part of the actinide molecular science competency development effort, the initial goal of this work is to synthesize and investigate several series of complexes, varying by actinide metal, ligand set, and oxidation state. We are examining the reactivity of plutonium and neptunium organometallic complexes to elucidate fundamental chemical parameters of the metals. These reactions will be compared to those of the known corresponding uranium complexes in order to recognize trends among the actinide elements and to document differences in chemical behavior

Actinides and rare earths complexation with adenosine phosphate nucleotides

International Nuclear Information System (INIS)

Mostapha, Sarah

2013-01-01

Organophosphorus compounds are important molecules in both nuclear industry and living systems fields. Indeed, several extractants of organophosphorus compounds (such as TBP, HDEHP) are used in the nuclear fuel cycle reprocessing and in the biological field. For instance, the nucleotides are organophosphates which play a very important role in various metabolic processes. Although the literature on the interactions of actinides with inorganic phosphate is abundant, published studies with organophosphate compounds are generally limited to macroscopic and / or physiological approaches. The objective of this thesis is to study the structure of several organophosphorus compounds with actinides to reach a better understanding and develop new specific buildings blocks. The family of the chosen molecules for this procedure consists of three adenine nucleotides mono, bi and triphosphate (AMP, adenosine monophosphate - ADP, adenosine diphosphate - ATP, adenosine triphosphate) and an amino-alkylphosphate (AEP O-phosphoryl-ethanolamine). Complexes synthesis was conducted in aqueous and weakly acidic medium (2.8-4) for several lanthanides (III) (Lu, Yb, Eu) and actinides (U (VI), Th (IV) and Am (III)). Several analytical and spectroscopic techniques have been used to describe the organization of the synthesized complexes: spectrometric analysis performed by FTIR and NMR were used to identify the functional groups involved in the complexation, analysis by ESI-MS and pH-metric titration were used to determine the solution speciation and EXAFS analyzes were performed on Mars beamline of the SOLEIL synchrotron, have described the local cation environment, for both solution and solid compounds. Some theoretical approaches of DFT were conducted to identify stable structures in purpose of completing the experimental studies. All solid complexes (AMP, ADP, ATP and AEP) have polynuclear structures, while soluble ATP complexes are mononuclear. For all synthesized complexes, it has been

Synthesis and Characterization of Novel Magnetite Nanoparticle Block Copolymer Complexes

OpenAIRE

Zhang, Qian

2007-01-01

Superparamagnetic Magnetite (Fe3O4) nanoparticles were synthesized and complexed with carboxylate-functionalized block copolymers, and aqueous dispersions of the complexes were investigated as functions of their chemical and morphological structures. The block copolymer dispersants possessed either poly(ethylene oxide), poly(ethylene oxide-co-propylene oxide), or poly(ethylene oxide-b-propylene oxide) outer blocks, and all contained a polyurethane center block with pendant carboxylate functi...

PAMAM Dendrimers as Potential Carriers of Gadolinium Complexes of Iminodiacetic Acid Derivatives for Magnetic Resonance Imaging

Directory of Open Access Journals (Sweden)

Magdalena Markowicz-Piasecka

2015-01-01

Full Text Available This is the first study describing the utilization of PAMAM dendrimers as delivery vehicles of novel magnetic resonance imaging (MRI contrast agents. The purpose of this paper was to establish the potential of G4 PAMAM dendrimers as carriers of gadolinium complexes of iminodiacetic acid derivatives and determine imaging properties of synthesized compounds in in vivo studies. Furthermore, we examined the influence of four synthesized complexes on the process of clot formation, stabilization, and lysis and on amidolytic activity of thrombin. Biodistribution studies have shown that the compounds composed of PAMAM G4 dendrimers and gadolinium complexes of iminodiacetic acid derivatives increase signal intensity preferably in liver in range of 59–116% in MRI studies which corresponds with the greatest accumulation of gadolinium after administration of the compounds. Synthesized compounds affect kinetic parameters of the proces of clot formation, its stabilization, and lysis. However, only one synthesized compound at concentration 10-fold higher than potential plasma concentrations contributed to the increase of general parameters such as the overall potential of clot formation and lysis (↑CLAUC and total time of the process (↑T. Results of described studies provide additional insight into delivery properties of PAMAM dendrimers but simultaneously underscore the necessity for further research.

New Route to Synthesize Surface Organometallic Complexes (SOMC): An Approach by Alkylating Halogenated Surface Organometallic Fragments

KAUST Repository

Hamieh, Ali Imad Ali

2017-01-01

The aim of this thesis is to explore new simpler and efficient routes for the preparation of surface organometallic complexes (SOMC) for the transformation of small organic molecules to valuable products. The key element in this new route relies on surface alkylation of various halogenated surface coordination complexes or organometallic fragments (SOMF).

New Route to Synthesize Surface Organometallic Complexes (SOMC): An Approach by Alkylating Halogenated Surface Organometallic Fragments

KAUST Repository

Hamieh, Ali Imad

2017-02-01

The aim of this thesis is to explore new simpler and efficient routes for the preparation of surface organometallic complexes (SOMC) for the transformation of small organic molecules to valuable products. The key element in this new route relies on surface alkylation of various halogenated surface coordination complexes or organometallic fragments (SOMF).

Synthesis, Characterization and Antibacterial Studies of N-(Benzothiazol-2-yl-4-chlorobenzenesulphonamide and Its Neodymium(III and Thallium(III Complexes

Directory of Open Access Journals (Sweden)

Lawrence Nnamdi Obasi

2017-02-01

Full Text Available N-(Benzothiazol-2-yl-4-chlorobenzenesulphonamide (NBTCS was synthesized by condensation reaction of 4-chlorobenzenesulphonyl chloride and 2-aminobenzothiazole in acetone under reflux. Neodymium(III and thallium(III complexes of the ligand were also synthesized. Both ligand and metal complexes were characterized using UV-Vis, IR, 1H- and 13C-NMR spectroscopies, elemental analysis and molar conductance measurement. IR studies revealed that the ligand is tridentate and coordinates to the metal ions through nitrogen and oxygen atoms of the sulphonamide group and nitrogen atom attached to benzothiazole ring. The neodymium(III complex displays a coordination number of eight while thallium(III complex displays a coordination number of six. The ligand and its complexes were screened in vitro for their antibacterial activities against Escherichia coli strains (E. coli 6 and E. coli 13, Proteus species, Staphylococcus aureus and Pseudomonas aeruginosa using the agar well diffusion technique. The synthesized compounds were found to be more active against the microorganisms screened relative to ciprofloxacin, gentamicin and co-trimoxazole.

Characterising the cellulose synthase complexes of cell walls

NARCIS (Netherlands)

Mansoori Zangir, N.

2012-01-01

One of the characteristics of the plant kingdom is the presence of a structural cell wall. Cellulose is a major component in both the primary and secondary cell walls of plants. In higher plants cellulose is synthesized by so called rosette protein complexes with cellulose synthases (CESAs) as

Some transition metal ions complexes of tricine (Tn and amino acids: pH-titration, synthesis and antimicrobial activity

Directory of Open Access Journals (Sweden)

M.E. Zayed

2014-12-01

Full Text Available Equilibrium studies have been carried out on complex formation of M(II (M = Co(II, Cu(II and Zn(II with tricine (Tn and L = amino acids in aqueous solution, at 25 °C and ionic strength of I = 0.1 M (NaNO3. The ternary complexes of amino acids are formed by simultaneous reactions. The concentration distribution of the complexes is evaluated. The solid complexes of [M(II–Tn–Histidine (Hist] have been synthesized and characterized by elemental analysis, infrared, magnetic and conductance measurements. The synthesized complexes have been screened for their antibacterial activities and the complexes show a significant antibacterial activity against four bacterial species: Staphylococcus aureus (Gram +ve, Streptococcus pyogenesr (Gram +ve, Serratia marcescens (Gram −ve and Escherichia coli (Gram −ve. The activity increases by increasing the concentration of the complexes.

Synthesis of complex compounds in the system [ReOG5]2--thiosemicarbazone acetone-Hg-acetone

International Nuclear Information System (INIS)

Amindzhanov, A.A.; Kurbanov, N.M.

1993-01-01

Present article is devoted to synthesis of complex compounds in the system [ReOG 5 ] 2- -thiosemicarbazone acetone-Hg-acetone. The literature data on complex compounds of various metals with thiosemicarbazone was summarized. The synthesis of complex compounds in the system [ReOG 5 ] 2- -thiosemicarbazone acetone-Hg-acetone was conducted. The complex compounds of rhenium with methyl ident thiosemicarbazone were synthesized.

Solid phase syntheses of oligoureas

Energy Technology Data Exchange (ETDEWEB)

Burgess, K.; Linthicum, D.S.; Russell, D.H.; Shin, H.; Shitangkoon, A.; Totani, R.; Zhang, A.J.; Ibarzo, J. [Texas A& M Univ., College Station, TX (United States)

1997-02-19

Isocyanates 7 were formed from monoprotected diamines 3 or 6, which in turn can be easily prepared from commercially available N-BOC- or N-FMOC-protected amino acid derivatives. Isocyanates 7, formed in situ, could be coupled directly to a solid support functionalized with amine groups or to amino acids anchored on resins using CH{sub 2}Cl{sub 2} as solvent and an 11 h coupling time at 25 {degree}C. Such couplings afforded peptidomimetics with an N-phthaloyl group at the N-terminus. The optimal conditions identified for removal of the N-phthaloyl group were to use 60% hydrazine in DMF for 1-3 h. Several sequences of amino acids coupled to ureas (`peptidic ureas`) and of sequential urea units (`oligoureas`) were prepared via solid phase syntheses and isolated by HPLC. Partition coefficients were measured for two of these peptidomimetics, and their water solubilities were found to be similar to the corresponding peptides. A small library of 160 analogues of the YGGFL-amide sequence was prepared via Houghten`s tea bag methodology. This library was tested for binding to the anti-{beta}-endorphin monoclonal antibody. Overall, this paper describes methodology for solid phase syntheses of oligourea derivatives with side chains corresponding to some of the protein amino acids. The chemistry involved is ideal for high-throughput syntheses and screening operations. 51 refs., 3 figs., 2 tabs.

Substitution of conventional high-temperature syntheses of inorganic compounds by near-room-temperature syntheses in ionic liquids

KAUST Repository

Groh, Matthias Friedrich

2013-01-01

The high-temperature syntheses of the low-valent halogenides P2I4, Te2Br, α-Te4I4, Te4(Al2Cl7)2, Te4(Bi6Cl20), Te8(Bi4Cl14),Bi8(AlCl4)2, Bi6Cl7,and Bi6Br7, as well as of WSCl4 andWOCl4 have been replaced by resource-efficient low-temperature syntheses in room temperature ionic liquids (RTILs). The simple one-pot syntheses generally do not require elaborate equipment such as twozone furnaces or evacuated silica ampoules. Compared to the published conventional approaches, reduction of reaction time (up to 80%) and temperature (up to 500 K) and, simultaneously, an increase in yield were achieved. In the majority of cases, the solid products were phase-pure. X-Ray diffraction on single crystals (redetermination of 11 crystal structures) has demonstrated that the quality of the crystals from RTILs is comparable to that of products obtained by chemical transport reactions. © 2013 Verlag der Zeitschrift für Naturforschung, Tübingen.

Phosphorescence Imaging of Living Cells with Amino Acid-Functionalized Tris(2-phenylpyridine)iridium(III) Complexes

NARCIS (Netherlands)

Steunenberg, P.; Ruggi, A.; Berg, van den N.S.; Buckle, T.; Kuil, J.; Leeuwen, van F.W.B.; Velders, A.H.

2012-01-01

A series of nine luminescent cyclometalated octahedral iridium(III) tris(2-phenylpyridine) complexes has been synthesized, functionalized with three different amino acids (glycine, alanine, and lysine), on one, two, or all three of the phenylpyridine ligands. All starting complexes and final

Study of new 113mIn-BAT complexes for myocardial imaging agents

International Nuclear Information System (INIS)

Zhu Lin; Liu Boli; Kojima, M.

1991-01-01

Some new BAT derivatives are designed and synthesized in order to find some ideal myocardial imaging agents. These ligands form pentacoordinated complexes with indium cation. The structures of ligand BAT-TE and complexes In-BAT-TE and In-BAT-ETE are determined by X-ray crystallography at first. Biodistribution shows that the higher lipophilicity of complex induces apparently higher myocardial accumulation. Up to date, complex B is the best 113m In-labeled myocardial imaging agent. It is also suited to 111 In

Bowl adamanzanes--bicyclic tetraamines: syntheses and crystal structures of complexes with cobalt(III) and chelating coordinated oxo-anions.

Science.gov (United States)

Broge, Louise; Søtofte, Inger; Jensen, Kristian; Jensen, Nicolai; Pretzmann, Ulla; Springborg, Johan

2007-09-14

Seven cobalt(III) complexes of the macrobicyclic tetraamine ligand [2(4).3(1)]adamanzane ([2(4).3(1)]adz) are reported along with the crystal structure of six of these complexes. The solid state and solution structures are discussed, and a detailed assignment of the NMR spectra of the sulfato complex is provided. Four of the seven complexes contain a chelate coordinating oxo-anion (sulfate, formiate, nitrate, carbonate). Equilibration of these species with the corresponding diaqua complex is generally slow. The rates of equilibration in 5 mol dm(-3) perchloric acid at 25 degrees C have been measured, yielding half lives of 20 min, 10 min and 3 h for the sulfato, formiato and carbonato species respectively. The corresponding reaction for the nitrato complex occurs with a half life of less than 3 min. The concentration acid dissociation constant for the Co([2(4).3(1)]adz)(HCO(3))(2+) ion has been measured to K(a) = 0.33 mol dm(-3) [25 degrees C, I = 2 mol dm(-3)] and K(a) = 0.15 mol dm(-3) [25 degrees C, I = 5 mol dm(-3)]. The propensity for coordination of sulfate was found to be large enough for a quantitative conversion of the carbonato complex to the sulfato complex to occur in 3 mol dm(-3) triflic acid containing a small sulfate contamination. On this basis the decarboxylation in 5 mol dm(-3) triflic acid of the corresponding cobalt(III) carbonato complex of the larger macrobicyclic tetraamine ligand [3(5)]adz was reinvestigated and found to lead to the sulfato complex as well. The difference in exchange rate of the oxo-anion ligands for the cobalt(III) complexes of the two adamanzane ligands is discussed and attributed to fundamental differences in the molecular structure where an inverted configuration of the secondary non-bridged amine groups is seen for the complexes of the larger [3(5)]adz ligand. The high affinity for chelating coordination of oxo-anions for these two cobalt(iii)-adamanzane-moieties is rationalised on basis of the N-Co-N angles. N

Nickel(II) and palladium(II) triphenylphosphine complexes incorporating tridentate Schiff base ligands: Synthesis, characterization and biocidal activities

Science.gov (United States)

Shabbir, Muhammad; Akhter, Zareen; Ashraf, Ahmad Raza; Ismail, Hammad; Habib, Anum; Mirza, Bushra

2017-12-01

Nickel(II) and palladium(II) triphenylphosphine complexes incorporating tridentate Schiff bases have been prepared and characterized by elemental analysis as well as by spectroscopic techniques (FTIR & NMR). The synthesized compounds were assessed to check their potential biocidal activity by using different biological assays (brine shrimp cytotoxicity, antimicrobial, antioxidant, antitumor and drug-DNA interaction). Results of brine shrimp cytotoxicity assay showed that ligand molecules are more bioactive than metal complexes with LD50 as low as 12.4 μg/mL. The prominent antitumor activity was shown by nickel complexes while the palladium complexes exhibited moderate activity. The synthesized compounds have shown high propensity for DNA binding either through intercalation or groove binding which represents the mechanism of antitumor effect of these compounds. Additionally, ligand molecules and nickel metal complexes showed significant antioxidant activity with IC50 values as low as 3.1 μg/mL and 18.9 μg/mL respectively while palladium complexes exhibited moderate activity. Moreover, in antimicrobial assays H2L1, Ni(L1)PPh3 and H2L3 showed dual inhibition against bacterial and fungal strains while for the rest of the compounds varying degree of activity was recorded against different strains. Overall comparison of results suggests that the synthesized compounds can be promising candidate for drug formulation and development.

Study on photophysical properties of Eu(III) complexes with aromatic β-diketones – Role of charge transfer states in the energy migration

Energy Technology Data Exchange (ETDEWEB)

Räsänen, Markus, E-mail: mpvras@utu.fi [Department of Chemistry, University of Turku, FIN-20014 Turku (Finland); Takalo, Harri [DHR Finland Oy, Innotrac Diagnostics, Biolinja 12, FIN-20750 Turku (Finland); Rosenberg, Jaana; Mäkelä, Joonas [Department of Biochemistry and Food Chemistry, University of Turku, FIN-20014 Turku (Finland); Haapakka, Keijo; Kankare, Jouko [Department of Chemistry, University of Turku, FIN-20014 Turku (Finland)

2014-02-15

We synthesized a set of aromatic β-diketones and measured the photophysical properties of their europium(III) complexes. According to these photophysical properties, the europium complexes can be divided into two groups: the complexes with or without the freely rotating amino-group (FRAG). On the basis of the experimental results, it can be concluded that in the FRAG complexes, the ligand-centered excitation energy is most probably transferred from a ligand to a coordinated europium via the intraligand charge transfer (ILCT) state. The temperature dependency of the lifetimes of the emissive {sup 5}D{sub 0} state revealed that in the FRAG complexes, the energy of the emissive {sup 5}D{sub 0} state is back-transferred to the ligand-to-metal charge transfer (LMCT) state and in the non-FRAG complexes, to the triplet state of the ligand. The most efficient complex synthesized was the europium complex of carbazole derivative L{sup 6} with the quantum yield of 47% and molar absorption coefficient of 70,400 M{sup −1}cm{sup −1}. -- Highlights: • We synthesized a set of substituted aromatic β-diketones and their Eu(III) complexes. • We measured the photophysical properties of these Eu(III) complexes. • Carbazole derivative of β-diketone forms the brightest Eu(III) complex. • The Jablonski diagrams proposed for the luminescence of these complexes.

Electron spin resonance of vanadium(4)-thallium(1) dithiocarbamate complexes

International Nuclear Information System (INIS)

Ivanov, A.V.; Solozhenkin, P.M.; Baratova, Z.R.; Klyashtornyj, V.B.; Uskov, V.Yu.

1990-01-01

Heteronuclear vanadium(4), thallium(1) dithiocarbanate complexes of the composition TlVO(Dtc) 3 and Tl 2 VO(Dtc) 4 under conditions of magnetic dilution were studied by ESR spectroscopy. Magnetically diluted complexes were prepared by coprecipitation from aqueous solutions of thallium(1) and oxovanadium(2) by solutions of sodium diethyldithiocarbamate, dibutyldithiocarbamate, hexamethylenedithiocarbamate, taken in superstoichiometric excess. Analysis of parameters of ESR spectra of the complexes synthesized shows that thallium atoms are not included in the first coordination sphere of oxovanadium(2), and chelate node VS 4 in thallium(1) complex lattice practically preserves its plane quadratic structure

Syntheses and evaluation of 68 Ga- and 153 Sm-labeled DOTA-conjugated bisphosphonate ligand for potential use in detection of skeletal metastases and management of pain arising from skeletal metastases.

Science.gov (United States)

Chakraborty, Sudipta; Goswami, Dibakar; Chakravarty, Rubel; Mohammed, Sahiralam Khan; Sarma, Haladhar Deb; Dash, Ashutosh

2018-05-05

This article reports the syntheses and evaluation of 68 Ga- and 153 Sm-complexes of a new DOTA (1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid)-conjugated geminal bisphosphonate, DOTA-Bn-SCN-BP, for their potential uses in the early detection of skeletal metastases by imaging and palliation of pain arising from skeletal metastases, respectively. The conjugate was synthesized in high purity following an easily adaptable three-step reaction scheme. Gallium-68- and 153 Sm-complexes were prepared in high yield (>98%) and showed excellent in vitro stability in phosphate-buffered saline (PBS) and human serum. Both the complexes showed high affinity for hydroxyapatite particles in in vitro binding study. In biodistribution studies carried out in normal Wistar rats, both the complexes exhibited rapid skeletal accumulation with almost no retention in any other major organ. The newly synthesized molecule DOTA-Bn-SCN-BP would therefore be a promising targeting ligand for the development of radiopharmaceuticals for both imaging skeletal metastases and palliation of pain arising out of it in patients with cancer when radiolabeled with 68 Ga and 153 Sm, respectively. A systematic comparative evaluation, however, showed that there was no significant improvement of skeletal accumulation of the 153 Sm-DOTA-Bn-SCN-BP complex over 153 Sm-DOTMP (1,4,7,10-tetraazacyclododecane-1,4,7,10-tetramethylenephosphonic acid) as the later itself demonstrated optimal properties required for an agent for bone pain palliation. © 2018 John Wiley & Sons A/S.

Operational Design that Synthesizes Art and Science

Science.gov (United States)

2011-05-04

FINAL 3. DATES COVERED (From - To) Feb - May 2011 4. TITLE AND SUBTITLE OPERATIONAL DESIGN THAT SYNTHESIZES ART AND SCIENCE 5a...TITLE AND SUBTITLE Operational Design That Synthesizes Art And Science 5a. CONTRACT NUMBER 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR...proponents of EBO view warfare as only a science and not a combination of art and science . 9 Another main point of contention centered on the term

Palladium(0) NHC complexes: a new avenue to highly efficient phosphorescence.

Science.gov (United States)

Henwood, Adam F; Lesieur, Mathieu; Bansal, Ashu K; Lemaur, Vincent; Beljonne, David; Thompson, David G; Graham, Duncan; Slawin, Alexandra M Z; Samuel, Ifor D W; Cazin, Catherine S J; Zysman-Colman, Eli

2015-05-01

We report the first examples of highly luminescent di-coordinated Pd(0) complexes. Five complexes of the form [Pd(L)(L')] were synthesized, where L = IPr, SIPr or IPr* NHC ligands and L' = PCy 3 , or IPr and SIPr NHC ligands. The photophysical properties of these complexes were determined in degassed toluene solution and in the solid state and contrasted to the poorly luminescent reference complex [Pd(IPr)(PPh 3 )]. Organic light-emitting diodes were successfully fabricated but attained external quantum efficiencies of between 0.3 and 0.7%.

Hydrolysis of Letrozole catalyzed by macrocyclic Rhodium (I) Schiff-base complexes.

Science.gov (United States)

Reddy, P Muralidhar; Shanker, K; Srinivas, V; Krishna, E Ravi; Rohini, R; Srikanth, G; Hu, Anren; Ravinder, V

2015-03-15

Ten mononuclear Rhodium (I) complexes were synthesized by macrocyclic ligands having N4 and N2O2 donor sites. Square planar geometry is assigned based on the analytical and spectral properties for all complexes. Rh(I) complexes were investigated as catalysts in hydrolysis of Nitrile group containing pharmaceutical drug Letrozole. A comparative study showed that all the complexes are efficient in the catalysis. The percent yields of all the catalytic reaction products viz. drug impurities were determined by spectrophotometric procedures and characterized by spectral studies. Copyright © 2014 Elsevier B.V. All rights reserved.

Colchiceine Complexes with Lithium, Sodium and Potassium Salts − Spectroscopic Studies

Directory of Open Access Journals (Sweden)

Joanna Kurek

2016-09-01

Full Text Available Colchiceine complexes with Li+, Na+ and K+ cations have been synthesized and studied by 1H and 13C NMR, FT-IR, FAB MS and UV-Vis. It has been shown that colchiceine forms stable complexes especially with lithium cation and the most stable structures of the complexes are those in which the acetamide groups are involved in the coordination process. The structures of the colchiceine complexes with Li+, Na+ and K+ cations are discussed in details. This work is licensed under a Creative Commons Attribution 4.0 International License.

Fully automated parallel oligonucleotide synthesizer

Czech Academy of Sciences Publication Activity Database

Lebl, M.; Burger, Ch.; Ellman, B.; Heiner, D.; Ibrahim, G.; Jones, A.; Nibbe, M.; Thompson, J.; Mudra, Petr; Pokorný, Vít; Poncar, Pavel; Ženíšek, Karel

2001-01-01

Roč. 66, č. 8 (2001), s. 1299-1314 ISSN 0010-0765 Institutional research plan: CEZ:AV0Z4055905 Keywords : automated oligonucleotide synthesizer Subject RIV: CC - Organic Chemistry Impact factor: 0.778, year: 2001

Template Syntheses, Crystal Structures and Supramolecular Assembly of Hexaaza Macrocyclic Copper(II) Complexes

International Nuclear Information System (INIS)

Kim, Taehyung; Kim, Ju Chang; Lough, Alan J.

2013-01-01

Two new hexaaza macrocyclic copper(II) complexes were prepared by a template method and structurally characterized. In the solid state, they were self-assembled by intermolecular interactions to form the corresponding supramolecules 1 and 2, respectively. In the structure of 1, the copper(II) macrocycles are bridged by a tp ligand to form a macrocyclic copper(II) dimer. The dimer extends its structure by intermolecular forces such as hydrogen bonds and C-H···π interactions, resulting in the formation of a double stranded 1D supramolecule. In 2, the basic structure is a monomeric copper(II) macrocycle with deprotonated imidazole pendants. An undulated 1D hydrogen bonded array is achieved through hydrogen bonds between imidazole pendants and secondary amines, where the imidazole pendants act as a hydrogen bond acceptor. The 1D hydrogen bonded supramolecular chain is supported by C-H···π interactions between the methyl groups of acetonitrile ligands and imidazole pendants of the copper(II) macrocycles. In both complexes, the introduction of imidazoles to the macrocycle as a pendant plays an important role for the formation of supramolecules, where they act as intermolecular hydrogen bond donors and/or acceptors, C-H···π and π-π interactions

Versatile lanthanide-azide complexes with azide/carboxylate/hydroxy mixed bridged chain exhibiting magnetic and luminescent properties

International Nuclear Information System (INIS)

Wang Haichao; Xue Min; Guo Qian; Zhao Jiongpeng; Liu Fuchen; Ribas, Joan

2012-01-01

Two new lanthanide-azide complexes, [Ln 2 (N 3 )(isonic) 2 (OH) 3 (Hisonic)(H 2 O)] n (Ln=Yb for 1 and Tb for 2, isonic=isonicotinate), were obtained in hydrothermal condition. X-ray diffraction analysis indicated the two complexes are isomorphic chain structure in which the Ln III ions are mixed bridged by the azide anions, hydroxyl anions and carboxylate groups of the isonicotinate ligands. Further studies indicated weak antiferromagnetic interactions between the Ln III ions in 1 and 2, and complex 2 exhibit green sensitized Luminescent character of Tb III ion. - Graphical abstract: Two new 1D lanthanide-azide complexes, [Ln 2 (N 3 )(isonic) 2 (OH) 3 (Hisonic)(H 2 O)] n (Ln=Yb III for 1 and Tb III for 2, isonic=isonicotinate), were synthesized by hydrothermal reaction and exhibit interesting magnetism and fluorescence properties. Highlights: ► The research provided a new method for synthesizing lanthanide-azide complexes. ► The complexes have an interesting azide/hydroxyl/carboxylate mixed bridged1D chain structure. ► The antiferromagnetic coupling between the complexes and 2 displays green luminescence.

Fluorido complexes of technetium

Energy Technology Data Exchange (ETDEWEB)

Mariappan Balasekaran, Samundeeswari

2013-07-04

Fluorine chemistry has received considerable interest during recent years due to its significant role in the life sciences, especially for drug development. Despite the great nuclear medicinal importance of the radioactive metal technetium in radiopharmaceuticals, its coordination chemistry with the fluorido ligand is by far less explored than that of other ligands. Up to now, only a few technetium fluorides are known. This thesis contains the synthesis, spectroscopic and structural characterization of novel technetium fluorides in the oxidation states ''+1'', ''+2'', ''+4'' and ''+6''. In the oxidation state ''+6'', the fluoridotechnetates were synthesized either from nitridotechnetic(VI) acid or from pertechnetate by using reducing agent and have been isolated as cesium or tetraethylammonium salts. The compounds were characterized spectroscopically and structurally. In the intermediate oxidation state ''+4'', hexafluoridotechnetate(IV) was known for long time and studied spectroscopically. This thesis reports novel and improved syntheses and solved the critical issues of early publications such as the color, some spectroscopic properties and the structure of this key compound. Single crystal analyses of alkali metal, ammonium and tetramethylammonium salts of hexafluoridotechnetate(IV) are presented. In aqueous alkaline solutions, the ammonium salt of hexafluoridotechnetate(IV) undergoes hydrolysis and forms an oxido-bridged dimeric complex. It is the first step hydrolysis product of hexafluoridotechnetate(IV) and was characterized by spectroscopic and crystallographic methods. Low-valent technetium fluorides with the metal in the oxidation states of ''+2'' or ''+1'' are almost unknown. A detailed description of the synthesis and characterization of pentafluoridonitrosyltechnetate(II) is presented. The

Synthesis, Cytotoxicity and Molecular Docking Study of Complexes Containing Thiazole Moiety

Directory of Open Access Journals (Sweden)

Mohammed Shafeeulla

2017-07-01

Full Text Available The ligand 5-methyl-2-phenyl-4-[(E-1,3-thiazol-2-yldiazenyl]-2,4-dihydro-3H-pyrazol-3-one (Dy has been synthesized by diazo coupling reactions of 5-methyl-2-phenyl- 2,4-dihydro-3H-pyrazol-3-one with 2-aminothiazole and ferric hydrogen sulfate (FHS, as a catalyst, under solvent-free conditions. A series of complexes of the ligand with Co(II, Ni(II, Cu(II, and Zn(II ions are synthesized and structurally characterized by 1H NMR, FTIR, and UV–Visible spectral techniques. The cytotoxic activity of the complexes and the uncoordinated ligand against human breast cancer (MCF-7 and chronic myelogenous leukemia cell line (human erythroleukemia (K-562 cell lines exhibits good viability in the range of 50.16–55.16% at a concentration of >100-110 µg/mL as compared to the inhibition in the untreated cells. Further, the metal complexes and ligand were screened against antibacterial strains of S. typhi, S. aureus, and E. coli. Both the cytotoxicity and antioxidant studies are correlated with computational docking analysis and powder XRD studies reviles that all complexes are in crystalline nature.

Silica functionalized Cu(II) acetylacetonate Schiff base complex: An efficient catalyst for the oxidative condensation reaction of benzyl alcohol with amines

Science.gov (United States)

Anbarasu, G.; Malathy, M.; Karthikeyan, P.; Rajavel, R.

2017-09-01

Silica functionalized Cu(II) acetylacetonate Schiff base complex via the one pot reaction of silica functionalized 3-aminopropyltriethoxysilane with acetyl acetone and copper acetate has been reported. The synthesized material was well characterized by analytical techniques such as FT-IR, UV-DRS, XRD, SEM-EDX, HR-TEM, EPR, ICP-AES and BET analysis. The characterization results confirmed the grafting of Cu(II) Schiff base complex on the silica surface. The catalytic activity of synthesized silica functionalized Cu(II) acetylacetonate Schiff base complex was evaluated through the oxidative condensation reaction of benzyl alcohol to imine.

Thermal stability and degradation kinetics of polyphenols and polyphenylenediamines enzymatically synthesized by horseradish peroxidase

Energy Technology Data Exchange (ETDEWEB)

Park, Hansol; Ryu, Keungarp [University of Ulsan, Ulsan (Korea, Republic of); Kwon, Oyul [Seoul National University of Science and Technology, Seoul (Korea, Republic of)

2015-09-15

Various substituted phenols and phenylenediamines were enzymatically polymerized by horseradish peroxidase in 80% (v/v) organic solvents-aqueous buffer (100 mM sodium acetate, pH 5) mixtures with H{sub 2}O{sub 2} as the oxidant. The thermal stability of the polymers was investigated by thermogravimetric analysis (TGA) and represented by the char yield (wt% of the initial polymer mass) after being heated at 800 .deg. C. Poly(p-phenylphenol) had the highest thermal stability among the synthesized polymers with a char yield of 47 wt%. The polymers containing amino groups such as poly(p-aminophenol) and polyphenylenediamines were also shown to possess high thermal stabilities. The activation energies for the thermal degradation of the polymers determined by derivative thermogravimetric analysis (DTG) using Horowitz-Metzger's pseudo-first-order kinetics were in the range between 23-65 kJ/mol and comparable to those of the chemically synthesized polymers. Dynamic structural changes of the enzymatically synthesized polymers upon heating were studied by differential scanning calorimetry (DSC). The DSC curves of poly(p-phenylphenol) showed a broad exothermic peaks between 150-250 .deg. C, indicating that the polymer undergoes complex structural transitions in the temperature range. On the other hand, the DSC curves of the poly(p-aminophenol) and the poly(p-phenylenediamine) which contain amino groups showed strong sharp endothermic peaks near 150 .deg. C, implying that these polymers possess homogeneous oriented structures which undergo a concerted structural disintegration upon heating.

Thermal stability and degradation kinetics of polyphenols and polyphenylenediamines enzymatically synthesized by horseradish peroxidase

International Nuclear Information System (INIS)

Park, Hansol; Ryu, Keungarp; Kwon, Oyul

2015-01-01

Various substituted phenols and phenylenediamines were enzymatically polymerized by horseradish peroxidase in 80% (v/v) organic solvents-aqueous buffer (100 mM sodium acetate, pH 5) mixtures with H 2 O 2 as the oxidant. The thermal stability of the polymers was investigated by thermogravimetric analysis (TGA) and represented by the char yield (wt% of the initial polymer mass) after being heated at 800 .deg. C. Poly(p-phenylphenol) had the highest thermal stability among the synthesized polymers with a char yield of 47 wt%. The polymers containing amino groups such as poly(p-aminophenol) and polyphenylenediamines were also shown to possess high thermal stabilities. The activation energies for the thermal degradation of the polymers determined by derivative thermogravimetric analysis (DTG) using Horowitz-Metzger's pseudo-first-order kinetics were in the range between 23-65 kJ/mol and comparable to those of the chemically synthesized polymers. Dynamic structural changes of the enzymatically synthesized polymers upon heating were studied by differential scanning calorimetry (DSC). The DSC curves of poly(p-phenylphenol) showed a broad exothermic peaks between 150-250 .deg. C, indicating that the polymer undergoes complex structural transitions in the temperature range. On the other hand, the DSC curves of the poly(p-aminophenol) and the poly(p-phenylenediamine) which contain amino groups showed strong sharp endothermic peaks near 150 .deg. C, implying that these polymers possess homogeneous oriented structures which undergo a concerted structural disintegration upon heating.

Syntheses, crystal structures, and properties of new metal-5-bromonicotinate coordination polymers

Energy Technology Data Exchange (ETDEWEB)

Li, Wenjie [College of Chemistry and Molecular Engineering, Zhengzhou University, Zhengzhou 450052 (China); Li, Guoting [Department of Environmental and Municipal Engineering, North China University of Water Conservancy and Electric Power, Zhengzhou 450011 (China); Lv, Lulu; Zhao, Hong [College of Chemistry and Molecular Engineering, Zhengzhou University, Zhengzhou 450052 (China); Wu, Benlai, E-mail: wbl@zzu.edu.cn [College of Chemistry and Molecular Engineering, Zhengzhou University, Zhengzhou 450052 (China)

2015-05-15

Four metal–5-bromonicotinate (Brnic) coordination polymers [Fe(Brnic){sub 2}(H{sub 2}O){sub 2}]{sub n} (1), [Ni(Brnic){sub 2}]{sub n} (2), [Ni(Brnic)(bpy)(H{sub 2}O){sub 2}]{sub n}·n(Brnic)·4.5nH{sub 2}O (3), and [Co{sub 2}(Brnic){sub 3}(bpy){sub 2}(OH)]{sub n}·nH{sub 2}O (4) have been synthesized and structurally characterized (bpy=4,4′-bipyridine). Complex 1 has corrugated (4,4) sheets formed by μ-Brnic ligands and planar nodes Fe(II). As for 2–4, they all built up from Brnic-bridged dinuclear subunits, but have very different structure features. Complex 2 is a twin-like polymer with (4,4) layers formed by twin paddle-wheel [Ni{sub 2}(Brnic){sub 4}] subunits. Through the bridge coordination of bpy ligands with dinuclear rings [Ni{sub 2}(Brnic){sub 2}] and trigons [Co{sub 2}(Brnic){sub 3}(OH)], 6{sup 3}-topological cationic layers with nanosized grids of 3 and chiral ladder-type double chains of 4 formed, respectively. Notably, halogen-related interactions play an important role in the formation of 3D metallosupermolecules 1–4. The thermostabilities of all compounds have been discussed in detail. Moreover, the magnetic investigations of 2 and 4 indicate that there exist antiferromagnetic interactions in the paddle-wheel [Ni{sub 2}(Brnic){sub 4}] and trigon [Co{sub 2}(Brnic){sub 3}(OH)] cores, respectively. - Highlights: • Four novel metal–5-bromonicotinate coordination polymers have been synthesized. • Notably, halogen-related interactions play an important role in the formation of 3D metallosupermolecules. • Antiferromagnetic interactions in nickel(II) paddle-wheel and cobalt(II) trigon cores were observed.

A frequency tracking synthesizer for beam diagnostic systems

International Nuclear Information System (INIS)

Peterson, D.; Marriner, J.

1991-01-01

In low and medium energy synchrotrons the beam revolution frequency changes by a large factor during the acceleration process. High production rates require that these machines cycle rapidly. In attempting to diagnose instabilities which develop during the acceleration process it is useful to be able to select some frequency segment between revolution harmonics for viewing. Most types of test equipment operating in the frequency domain, such as spectrum analyzers and network analyzers, are not suited to making direct measurements on such rapidly sweeping signals. Ideally, one would want to set the frequency frame of reference to the spot in the accelerating revolution harmonic domain where the measurements are to be made. A scheme using a direct digital synthesizer (DDS) was developed to provide this moving reference frame. This paper describes a synthesizer scheme combining digital and analog synthesizer techniques to allow tracking of signals during acceleration. Virtually any ratio of synthesizer to beam revolution frequency may be generated by this scheme. Details of hardware and measurement results are presented

Schiff base transition metal complexes for Suzuki–Miyaura cross

Indian Academy of Sciences (India)

Schiff base ligand and its complex with iron (Fe), cobalt (Co), nickel (Ni) and copper (Cu) ions were synthesized using 4-aminoacetophenone and salicylaldehyde and characterized. FTIR spectrum shows that bidentate coordination of metal ions with ligand where O, N are electron donating sites of azomethine group.

Three new Ag(I) coordination architectures based on mixed ligands: Syntheses, structures and photoluminescent properties

Energy Technology Data Exchange (ETDEWEB)

Li, Yamin, E-mail: liyamin@henu.edu.cn [Institute of Molecular and Crystal Engineering, College of Chemistry and Chemical Engineering, Henan University, Kaifeng, Henan 475004 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Xiao, Changyu; Li, Shu; Chen, Qi; Li, Beibei; Liao, Qian; Niu, Jingyang [Institute of Molecular and Crystal Engineering, College of Chemistry and Chemical Engineering, Henan University, Kaifeng, Henan 475004 (China)

2013-04-15

Three new silver (I) coordination complexes, [Ag{sub 2}(1,2-bdc)(phdat)]{sub n} (1), [Ag{sub 2}(NO{sub 2}-bdc)(phdat)]{sub n} (2), [Ag{sub 4}(nta){sub 3}(phdat)NO{sub 3}]{sub n} (3) (1,2-bdc=phthalic acid dianion, NO{sub 2}-bdc=5-nitro-1,3-benzenedicarboxylic acid dianion, nta=nicotinic acid anion, phdat=2,4-diamine-6-phenyl-1,3,5-triazine) have been hydrothermally synthesized by the reactions of silver nitrate and phdat with the homologous ligands 1,2-H{sub 2}bdc, NO{sub 2}-H{sub 2}bdc, and Hnta, respectively, and characterized by single-crystal X-ray diffractions, IR spectra, elemental analyses thermogravimetric analyses (TGA). The compound 1 exhibits a chiral 3D network with cbs/CrB self-dual topological net, which contains two kinds of single helical chains. For compound 2, the 3D network is comprised of two kinds of similar 2D sheets with the topological symbol of sql-type packed in AABBAA mode by Ag–N/O weakly contacts. And compound 3 has 2D double layer architecture, consisting of the 2D plane with hcb-type topological symbol connected by Ag–O weakly coordinations. The photoluminescent properties associated with the crystal structures of three compounds have also been measured. - Graphical abstract: Three new silver(I) coordination complexes 1–3 have been synthesized and characterized by single-crystal X-ray diffractions, IR spectra, elemental analyses, thermogravimetric analyses (TGA) and photoluminescent spectra. Highlights: ► The compound 1 exhibits a novel chiral 3D network with two kinds of single helical chains. ► 3D or 2D new Ag coordination complexes. ► The photoluminescent properties have been measured.

Bowl adamanzanes-bicyclic tetraamines: syntheses and crystal structures of complexes with cobalt(III) and chelating coordinated oxo-anions

DEFF Research Database (Denmark)

Broge, Louise; Søtofte, Inger; Jensen, Kristian

2007-01-01

complex is provided. Four of the seven complexes contain a chelate coordinating oxo-anion ( sulfate, formiate, nitrate, carbonate). Equilibration of these species with the corresponding diaqua complex is generally slow. The rates of equilibration in 5 mol dm(-3) perchloric acid at 25 degrees C have been...

Partial strands synthesizing leads to inevitable aborting and complicated products in consecutive polymerase chain reactions (PCRs)

Institute of Scientific and Technical Information of China (English)

LUO Rui; ZHANG DaMing

2007-01-01

Various abnormal phenomena have been observed during PCR so far. The present study performed a series of consecutive PCRs (including many rounds of re-amplification continuously) and found that the abortion of re-amplification was inevitable as long as a variety of complicated product appeared.The aborting stages varied, according to the lengths of targets. Longer targets reached the abortion earlier than the shorter ones, marked by appearance of the complex that was immobile in electrophoresis. Denatured gel-electrophoresis revealed that the complex was mainly made up of shorter or partially synthesized strands, together with small amounts of full-length ones. Able to be digested by S1 nuclease but unable by restriction endonucleases (REs), the complex was proved to consist of both single regions and double-helix regions that kept the complex stable thermodynamically. Simulations gave evidence that partial strands, even at lower concentration, could disturb re-amplification effectively and lead to the abortion of re-amplifications finally. It was pointed out that the partial strands formed chiefly via polymerase's infidelity, and hence the solution to lighten the abnormality was also proposed.

Synthesis, characterization and anticancer activity of gold(I) complexes that contain tri-tert-butylphosphine and dialkyl dithiocarbamate ligands

KAUST Repository

Altaf, Muhammad

2015-03-10

Two new gold(I) complexes that contain tri-ter-butylphosphine and dialkyl dithiocarbamate ligands were synthesized and characterized by FTIR, NMR spectroscopy, Cyclic voltammetry, elemental analysis and X-ray diffraction. The in vitro cytotoxicity of both complexes was examined against A549 (lung cancer), MCF7 (breast cancer), and HeLa (cervical cancer) human cancer cell lines. Both complexes exhibit very strong in vitro cytotoxic effects against A549, MCF7 and HeLa cell lines. The screening of the cytotoxic activity based on IC50 data against the A549, MCF7, and HeLa lines shows that the synthesized gold(I) complexes are highly effective, particularly against HeLa cancer cell line. Based on IC50 data, the cytotoxic activity of both complexes is better than well-known commercial anticancer drug cisplatin against all the three cancer lines tested.

Synthesis, Spectroscopic Characterization and Biological Activities of Transition Metal Complexes Derived from a Tridentate Schiff Base

Directory of Open Access Journals (Sweden)

J. Senthil Kumaran

2013-01-01

Full Text Available A new series of Cu (II, Ni (II, Co (II and Zn (II complexes have been synthesized from the Schiff base derived from 4-hydroxy-3-methoxybenzylidine-4-aminoantipyrine and 2-aminophenol. The structural features have been determined from their elemental analysis, magnetic susceptibility, molar conductance, Mass, IR, UV-Vis, 1H-NMR, 13C-NMR and ESR spectral studies. The redox behavior of the copper complex has been studied by cyclic voltammetry. The data confirm that the complexes have composition of ML2 type. The electronic absorption spectral data of the complexes propose an octahedral geometry around the central metal ion. All the metal complexes with DNA structure were guided by the presence of inter-molecular C–H⋯O and C–H⋯N hydrogen bonds. The biological activity of the synthesized compounds were tested against the bacterial species such as Bacillus subtilis, Staphylococcus aureus, Proteus vulgaris and fungal species such as Candida albicans by the well-diffusion method.

Synthesizing Earth's geochemical data for hydrogeochemical analysis

Science.gov (United States)

Brantley, S. L.; Kubicki, J.; Miller, D.; Richter, D.; Giles, L.; Mitra, P.

2007-12-01

For over 200 years, geochemical, microbiological, and chemical data have been collected to describe the evolution of the surface earth. Many of these measurements are data showing variations in time or in space. To forward predict hydrologic response to changing tectonic, climatic, or anthropogenic forcings requires synthesis of these data and utilization in hydrogeochemical models. Increasingly, scientists are attempting to synthesize such data in order to make predictions for new regions or for future time periods. However, to make such complex geochemical data accessible requires development of sophisticated cyberinfrastructures that both invite uploading as well as usage of data. Two such cyberinfrastructure (CI) initiatives are currently developing, one to invite and promote the use of environmental kinetics data (laboratory time course data) through ChemxSeer, and the other to invite and promote the use of spatially indexed geochemical data for the Earth's Critical Zone through CZEN.org. The vision of these CI initiatives is to provide cyber-enhanced portals that encourage domain scientists to upload their data before publication (in private cyberspace), and to make these data eventually publicly accessible (after an embargo period). If the CI can be made to provide services to the domain specialist - e.g. to provide data analysis services or data comparison services - we envision that scientists will upload data. In addition, the CI can promote the use and comparison of datasets across disciplines. For example, the CI can facilitate the use of spatially indexed geochemical data by scientists more accustomed to dealing with time-course data for hydrologic flow, and can provide user-friendly interfaces with CI established to facilitate the use of hydrologic data. Examples of the usage of synthesized data to predict soil development over the last 13ky and its effects on active hydrological flow boundaries in surficial systems will be discussed for i) a N

Synthesis, spectral characterisation, morphology, biological activity and DNA cleavage studies of metal complexes with chromone Schiff base

Directory of Open Access Journals (Sweden)

P. Kavitha

2016-07-01

Full Text Available Cu(II, Co(II, Ni(II and Zn(II complexes have been synthesized using 3-((pyridine-2-yliminomethyl-4H-chromen-4-one as a ligand derived from 3-formyl chromone and 2-amino pyridine. All the complexes were characterised by analytical, conductivity, IR, electronic, magnetic, ESR, thermal, powder XRD and SEM studies. The analytical data revealed that the metal to ligand molar ratio is 1:2 in all the complexes. Molar conductivity data indicates that all the complexes are neutral in nature. On the basis of magnetic and electronic spectral data, octahedral geometry is proposed for all the complexes. Thermal behaviour of the synthesized complexes indicates the coordinated and lattice water molecules are present in the complexes. The X-ray diffraction data suggest a triclinic system for all compounds. Different surface morphologies were identified from SEM micrographs. All metal complexes exhibit fluorescence. The antimicrobial and nematicidal activity data show that metal complexes are more potent than the parent ligand. The DNA cleavage activity of the ligand and its metal complexes were observed in the presence of H2O2.

A curcumin-based TPA four-branched copper(II) complex probe for in vivo early tumor detection

Energy Technology Data Exchange (ETDEWEB)

Pi, Zongxin [Department of Chemical and Chemical Engineering, Hefei Normal University, Hefei 230001 (China); Wang, Jiafeng; Jiang, Bo [Department of Pharmacy, Anhui University of Chinese Medicine, Hefei 230038 (China); Cheng, Gang [Department of Chemical and Chemical Engineering, Hefei Normal University, Hefei 230001 (China); Zhou, Shuangsheng, E-mail: zshuangsheng@126.com [Department of Pharmacy, Anhui University of Chinese Medicine, Hefei 230038 (China); Center of Modern Experimental Technology, Anhui University, Hefei 230038 (China)

2015-01-01

A multibranched Cu(II) complex CuL{sub 2} curcumin-based was synthesized and characterized by single-crystal X-ray diffraction analysis. The photophysical properties of the complex have been investigated both experimentally and theoretically. The results show that the target complex exhibits higher quantum yield and larger two-photon absorption (TPA) cross-section in the near infrared (NIR) region compared with its free ligand. The cell imaging studies in vitro and in vivo reveal that the complex shows good photostability and excellent tumor targeting capability to tested cancerous cells, which can be potentially used for early tumor detection. - Graphical abstract: A multibranched Cu(II) complex was prepared from curcumin. The photophysical properties of the obtained complex have been investigated. The results exhibit that the complex has high capability to test cancerous cells and can distinguish between the cancerous and noncancerous cells, which should be potentially used for early tumor detection. - Highlights: • A novel multi-branched copper complex was synthesized. • The obtained compounds exhibited obvious TPA in high polar solvents. • The complex is a low toxicity at low-micromolar concentrations. • The complex exhibits larger TPA cross-section and brighter TPF imaging. • The complex has excellent targeting capability to tested cancerous cells.

Microstructural and optical properties of Ca and Cr doped cobalt ferrite nanoparticles synthesized by auto combustion

Science.gov (United States)

Agrawal, Shraddha; Parveen, Azra; Azam, Ameer

2018-05-01

The Ca and Cr doped cobalt ferrite nanoparticles (Co0.8Ca0.2) (Fe0.8 Cr0.2)2O4 were synthesized by auto combustion method. Microstructural studies were carried out by X-ray diffraction (XRD). The crystalline size of synthesized nanoparticles as determined by the XRD was found to be 17.6 nm. These structural studies suggest that the crystal system remains spinal even with the doping of calcium and chromium. Optical properties of Ca and Cr doped cobalt ferrite were studied by UV-visible technique in the range of 200-800 nm. The energy band gap was calculated with the help of Tauc relationship. Ca and Cr doped cobalt ferrite annealed at 600°C exhibit significant dispersion in complex permeability. The dielectric constant and dielectric loss of cobalt ferrite were studied as a function of frequency and were explained on the basis of Koop's theory based on Maxwell Wagner two layer models and electron hopping.

Acousto-optics bandwidth broadening in a Bragg cell based on arbitrary synthesized signal methods.

Science.gov (United States)

Peled, Itay; Kaminsky, Ron; Kotler, Zvi

2015-06-01

In this work, we present the advantages of driving a multichannel acousto-optical deflector (AOD) with a digitally synthesized multifrequency RF signal. We demonstrate a significant bandwidth broadening of ∼40% by providing well-tuned phase control of the array transducers. Moreover, using a multifrequency, complex signal, we manage to suppress the harmonic deflections and return most of the spurious energy to the main beam. This method allows us to operate the AOD with more than an octave of bandwidth with negligible spurious energy going to the harmonic beams and a total bandwidth broadening of over 70%.

Synthesis and X-ray structure of the dysprosium(III) complex derived ...

African Journals Online (AJOL)

Synthesis and X-ray structure of the dysprosium(III) complex derived from the ligand 5-chloro-1 ... Bulletin of the Chemical Society of Ethiopia ... synthesized and its crystal structure determined by single X-ray diffraction at room temperature.

Beryllium(II), manganese(II) and uranyl(VI)-salicylamide complexes

Energy Technology Data Exchange (ETDEWEB)

Maurya, P L; Agarwala, B V; Dey, A K [Allahabad Univ. (India)

1977-01-01

The preparation, composition, general properties and i.r. absorption spectra of the solid chelates formed by salicylamide with beryllium(II), manganese(II) and uranyl(VI) are described. The complexes have been synthesized by refluxing a mixture of ethanolic solutions of the reactants (metal:ligand :: 1:2) for several hours in the presence of alkali. Attempts to isolate the complexes by the interaction of ethanolic solutions of the metal salts and the ligand in the absence of alkali did not succeed.

Spectroscopic and molecular docking studies on the interaction of human serum albumin with copper(II) complexes

Science.gov (United States)

Guhathakurta, Bhargab; Pradhan, Ankur Bikash; Das, Suman; Bandyopadhyay, Nirmalya; Lu, Liping; Zhu, Miaoli; Naskar, Jnan Prakash

2017-02-01

Two osazone based ligands, butane-2,3-dione bis(2‧-pyridylhydrazone) (BDBPH) and hexane-3,4-dione bis(2‧-pyridylhydrazone) (HDBPH), were synthesized out of the 2:1 M Schiff base condensation of 2-hydrazino pyridine respectively with 2,3-butanedione and 3,4-hexanedione. The X-ray crystal structures of both the ligands have been determined. The copper(II) complex of HDBPH has also been synthesized and structurally characterized. HDBPH and its copper(II) complex have thoroughly been characterized through various spectroscopic and analytical techniques. The X-ray crystal structure of the copper complex of HDBPH shows that it is a monomeric Cu(II) complex having 'N4O2' co-ordination chromophore. Interaction of human serum albumin (HSA) with these ligands and their monomeric copper(II) complexes have been studied by various spectroscopic means. The experimental findings show that the ligands as well as their copper complexes are good HSA binders. Molecular docking investigations have also been done to unravel the mode of binding of the species with HSA.

Synthesis, crystal structure and bioactivity of manganese complexes with asymmetric chiral Schiff base

Science.gov (United States)

Zhang, Enfeng; Wei, Yi; Huang, Fuping; Yu, Qing; Bian, Hedong; Liang, Hong; Lei, Fuhou

2018-03-01

A couple of chiral unsymmtrical Schiff base ligands, (1R,2R) (-)chxn (salH) (naftalH) and (1S,2S) (-)chxn (salH) (naftalH) had been synthesized by the condensation of salicylaldehyde and 2-hydroxy-1-naphthaldehyde with two isomers of (1R,2R)-trans-1,2-cyclohexanediamin and (1S,2S)-trans-1,2-cyclohexanediamin, respectively. At the same time, two manganese complexes have been synthesized and fully characterized by FT-IR spectrum, elemental analyses, single crystal X-ray diffraction. The interaction of the two Mn (III) complexes with bovine serum albumin (BSA) was investigated by spectroscopic techniques. The result reveals that the complexes can strongly quench the intrinsic fluorescence of BSA through a static quenching mechanism. The binding constant and binding mode has been determined. The secondary structure and the amino acid residues microenvironment of BSA change in the presence of these complexes. SOD-like activity and ABTS free radical scavenging ability were also studied. The antioxidant capacity of the compounds showed that the complexes and their corresponding BSA adducts showed some SOD activity. The results of ABTS free radical scavenging showed that the activity of the BSA adduct was more obvious than that of the complex.

A structurally characterized organometallic plutonium(IV) complex

Energy Technology Data Exchange (ETDEWEB)

Apostolidis, Christos; Walter, Olaf [European Commission, Joint Research Centre, Directorate G - Nuclear Safety and Security, Karlsruhe (Germany); Vogt, Jochen; Liebing, Phil; Edelmann, Frank T. [Chemisches Institut, Otto-von-Guericke-Universitaet Magdeburg (Germany); Maron, Laurent [Laboratoire de Physique et Chimie des Nanoobjets (LPCNO), Universite de Toulouse/INSA/CNRS (UMR5215), Toulouse (France)

2017-04-24

The blood-red plutonocene complex Pu(1,3-COT'')(1,4-COT'') (4; COT''=η{sup 8}-bis(trimethylsilyl)cyclooctatetraenyl) has been synthesized by oxidation of the anionic sandwich complex Li[Pu(1,4-COT''){sub 2}] (3) with anhydrous cobalt(II) chloride. The first crystal structure determination of an organoplutonium(IV) complex revealed an asymmetric sandwich structure for 4 where one COT'' ring is 1,3-substituted while the other retains the original 1,4-substitution pattern. The electronic structure of 4 has been elucidated by a computational study, revealing a probable cause for the unexpected silyl group migration. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

Method of synthesizing pyrite nanocrystals

Science.gov (United States)

Wadia, Cyrus; Wu, Yue

2013-04-23

A method of synthesizing pyrite nanocrystals is disclosed which in one embodiment includes forming a solution of iron (III) diethyl dithiophosphate and tetra-alkyl-ammonium halide in water. The solution is heated under pressure. Pyrite nanocrystal particles are then recovered from the solution.

Zr (IV COMPLEXES OF SOME NITROGEN-OXYGEN DONOR LIGANDS (SEMICARBAZONES & SALICYLALDAZINE

Directory of Open Access Journals (Sweden)

Z F DAWOOD

2002-06-01

Full Text Available Complexes containing mixed ligands of zirconium (IV have been synthesized by the reaction of zirconium (IV nitrate (Zr(NO34, 5H2O with salicylaldazine (SAH2 and semicarbazone ligands benzaldehyde semicarbazone (BSCH, 4-methoxybenzaldehyde semicarbzone (MBSCH, 2-chlorobenzaldehyde semicrbazone (CISCH and cinnamaldehyde semicarbazone (CinSCH forming complexes of the type [Zr2(SAH2(SCH2](NO38 and [Zr2(SA2 (SC2](NO32 in neutral and basic medium respectively. The ligands and their complexes are characterized physico-chemically.

Catalytic Hydroamination of Alkynes and Norbornene with Neutral and Cationic Tantalum Imido Complexes

Science.gov (United States)

Anderson, Laura L.; Arnold, John; Bergman, Robert G.

2005-01-01

Several tantalum imido complexes have been synthesized and shown to efficiently catalyze the hydroamination of internal and terminal alkynes. An unusual hydroamination/hydroarylation reaction of norbornene catalyzed by a highly electrophilic cationic tantalum imido complex is also reported. Factors affecting catalyst activity and selectivity are discussed along with mechanistic insights gained from stoichiometric reactions. PMID:15255680

1. Mono([8]annulene)Uranium(4) half-sandwich complexes, 2. Novel syntheses of symmetrically substituted cyclooctatetetraenes

International Nuclear Information System (INIS)

Boussie, T.R.

1991-10-01

A reproducible, high-yield synthesis of mono([8]annulene)uranium(4)dichloride (1) is reported, along with the X-ray crystal structural of the bis(pyridine) adduct. Metathesis reactions of the half-sandwich complex 1 with a variety of simple alkyl and alkoxy reagents failed to generate any isolable mono-ring complexes. Reactions of 1 with polydentate, delocalized anions did produce stable derivatives, including mono([8]annulene)uranium(4)bis(acetylacetonate) (4). An X-ray crystal structure of 4 is reported

1. Mono([8]annulene)Uranium(4) half-sandwich complexes, 2. Novel syntheses of symmetrically substituted cyclooctatetetraenes

Energy Technology Data Exchange (ETDEWEB)

Boussie, Thomas Richard [Univ. of California, Berkeley, CA (United States)

1991-10-01

A reproducible, high-yield synthesis of mono([8]annulene)uranium(4)dichloride (1) is reported, along with the X-ray crystal structural of the bis(pyridine) adduct. Metathesis reactions of the half-sandwich complex 1 with a variety of simple alkyl and alkoxy reagents failed to generate any isolable mono-ring complexes. Reactions of 1 with polydentate, delocalized anions did produce stable derivatives, including mono([8]annulene)uranium(4)bis(acetylacetonate) (4). An X-ray crystal structure of 4 is reported.

1. Mono((8)annulene)Uranium(4) half-sandwich complexes, 2. Novel syntheses of symmetrically substituted cyclooctatetetraenes

Energy Technology Data Exchange (ETDEWEB)

Boussie, T.R.

1991-10-01

A reproducible, high-yield synthesis of mono((8)annulene)uranium(4)dichloride (1) is reported, along with the X-ray crystal structural of the bis(pyridine) adduct. Metathesis reactions of the half-sandwich complex 1 with a variety of simple alkyl and alkoxy reagents failed to generate any isolable mono-ring complexes. Reactions of 1 with polydentate, delocalized anions did produce stable derivatives, including mono((8)annulene)uranium(4)bis(acetylacetonate) (4). An X-ray crystal structure of 4 is reported.

Bimetallic oxamato complexes synthesized into mesoporous matrix as precursor to tunable nanosized oxide

Energy Technology Data Exchange (ETDEWEB)

Kalinke, Lucas H.G. [Instituto de Química, Universidade Federal de Goiás—UFG, Goiânia, GO 74001-970 (Brazil); Instituto Federal de Goiás—IFG, Anápolis, GO (Brazil); Stumpf, Humberto O. [Departamento de Química, Instituto de Ciências Exatas, Universidade Federal de Minas Gerais—UFMG, Belo Horizonte, MG (Brazil); Mazali, Italo O. [Instituto de Química, Universidade Estadual de Campinas—UNICAMP, Campinas, SP (Brazil); Cangussu, Danielle, E-mail: danielle_cangussu@ufg.br [Instituto de Química, Universidade Federal de Goiás—UFG, Goiânia, GO 74001-970 (Brazil)

2015-10-15

Highlights: • The bimetallic oxamato complexes as single-source precursor. • We prepared into a porous silica glass tunable nanosized oxide powders. • X-ray diffraction shows the formation of CeO{sub 2}/CuO and spinel cobaltite. • The different number of IDC allows control of the nanoparticle size. - Abstract: The bimetallic complexes were employed to prepare into a porous silica glass tunable nanosized oxide powders through the single source precursor (SSP) method. These materials were prepared by first anchoring of [Cu(opba)]{sup 2−} [opba = ortho-phenylenebis(oxamato)], second by reaction in situ with second metal [Co(II) or Ce(III)] and followed by a thermal treatment. The different number of impregnation–decomposition cycles (IDC) allows control of the nanoparticle size. X-ray diffraction shows the formation of mixture CeO{sub 2}–CuO and spinel copper cobaltite. Raman spectroscopy confirmed the formation of such phases. Transmission electron microscopy images revealed that spinel cobaltite particles (8 IDC) present a mean size of about 9 nm, whereas for the CeO{sub 2}–CuO phase the particle diameters are 4 nm (2 IDC) and 8 nm (6 IDC). For CeO{sub 2}–CuO the diffuse reflectance spectroscopy indicates a consistent red shift in band gap from 3.41 to 2.87 eV with increasing of particle size due to quantum confinement effect.

Oxovanadium(IV) complexes of non-steroidal anti-inflammatory drugs: synthesis, spectroscopy, and antimicrobial activity

International Nuclear Information System (INIS)

Muhammad, N.; Ali, S.; Shahzadi, S.; Khan, A.N.

2008-01-01

Oxovanadium(IV) complexes with four different non-steroidal anti-inflammatory drugs have been synthesized. These complexes were characterized by different analytical techniques such as CHN, IR, UV-Vis spectroscopy, and mass spectrometry. The IR data show the bidentate nature of the ligands and reveal hexacoordinate geometry in the solid state. The complexes were tested for their biological activity against six different bacterial strains and plant pathogens, and all complexes showed good biological activity with few exceptions [ru

Antimony(3) ethylenediaminetetraacetate complexes with single- and doubly charged cations

International Nuclear Information System (INIS)

Davidovich, R.L.; Logvinova, V.B.; Kajdalova, T.A.

1998-01-01

The antimony(3) ethylenediaminetetraacetate complexes with alkaline and bivalent metals cations of the M + Sb(Edta) · H 2 O (M + = K, Rb, Cs, NH 4 ), M 2+ [Sb(Edta)] 2 · 8H 2 O (M 2+ = Mg, Ca, Sr, Co, Cd) composition are synthesized. Roentgenographic and IR-spectroscopic characteristics of the synthesized substances are determined. Two groups of the isostructural compounds: M + Sb(Edta) · H 2 O (M + = K, Rb, NH 4 ) and M 2+ [Sb(Edta)] 2 · 8H 2 O (M 2+ = Mg, Ca, Sr, Mn, Co, Cd) are established [ru

Synthesis, characterization and luminescent properties of lanthanide complexes with an unsymmetrical tripodal ligand

Energy Technology Data Exchange (ETDEWEB)

Yan Zhenzhong [State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China); Tang Yu [State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China)], E-mail: tangyu@lzu.edu.cn; Liu Weisheng; Tan Minyu [State Key Laboratory of Applied Organic Chemistry, College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China)

2008-09-15

Solid complexes of lanthanide nitrates with a new unsymmetrical tripodal ligand, bis[(2'-benzylaminoformyl)phenoxyl)ethyl](ethyl)amine (L) have been synthesized and characterized by elemental analysis, infrared spectra and molar conductivity measurements. At the same time, the luminescent properties of the Sm(III), Eu(III), Tb(III) and Dy(III) nitrate complexes in solid state were also investigated. Under the excitation of UV light, these complexes exhibited characteristic emission of central metal ions.

Phenoxo bridged dinuclear Zn(II) Schiff base complex as new precursor for preparation zinc oxide nanoparticles: Synthesis, characterization, crystal structures and photoluminescence studies

Energy Technology Data Exchange (ETDEWEB)

Saeednia, S., E-mail: sami_saeednia@yahoo.com [Department of Chemistry, Faculty of Science, Vali-e-Asr University of Rafsanjan, Rafsanjan 77188-97111 (Iran, Islamic Republic of); Iranmanesh, P. [Department of physics, Faculty of Science, Vali-e-Asr University of Rafsanjan, Rafsanjan 77188-97111 (Iran, Islamic Republic of); Ardakani, M. Hatefi; Mohammadi, M.; Norouzi, Gh. [Department of Chemistry, Faculty of Science, Vali-e-Asr University of Rafsanjan, Rafsanjan 77188-97111 (Iran, Islamic Republic of)

2016-06-15

Highlights: • A novel nano-scale Zn(II) complex was synthesized by solvothermal method. • Chemical structure of the nanostructures was characterized as well as bulk complex. • The photoluminescence property of the complex was investigated at room temperature. • The thermogravimetry and differential thermal analysis were carried out. • Thermal decomposition of the nanostructures was prepared zinc oxide nanoparticles. - Abstract: Nanoparticles of a novel Zn(II) Schiff base complex, [Zn(HL)NO{sub 3}]{sub 2} (1), (H{sub 2}L = 2-[(2-hydroxy-propylimino) methyl] phenol), was synthesized by using solvothermal method. Shape, morphology and chemical structure of the synthesized nanoparticles were characterized by scanning electron microscopy (SEM), X-ray powder diffraction (XRD), Fourier Transform Infrared Spectoscopy (FT-IR) and UV–vis spectroscopy. Structural determination of compound 1 was determined by single-crystal X-ray diffraction. The results were revealed that the zinc complex is a centrosymmetric dimer in which deprotonated phenolates bridge the two five-coordinate metal atoms and link the two halves of the dimer. The thermal stability of compound 1 was analyzed by thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC). The effect of the initial substrates concentration and reaction time on size and morphology of compound 1 nanostructure was investigated as well. Furthermore, the luminescent properties of the complex 1 were examined. ZnO nanoparticles with diameter between 15 and 20 nm were simply synthesized by solid-state transformation of compound 1 at 700 °C.

"Synthesizing Proteins”, the game: Proposal and evaluation of an educational tool

Directory of Open Access Journals (Sweden)

Julio Cesar Queiroz de Carvalho

2014-08-01

Full Text Available Educational games have been recommended by curriculum guides for biology teaching because they stimulate and promote group activities and foster spontaneous and creative development of students. The use of materials and diversified teaching strategies can facilitate the study of topics such as proteins and their relationship to DNA and RNA, which have some complexity and require a high level of abstraction. In this context we developed the game "Synthesizing Proteins", aimed at high school. The game promotes student recognition, use and interpretation of a meaningful and representative model of a biological system and can assist in developing the skills necessary for research, and scientific and technological understanding. The game comprises of a board containing a drawing of a eukaryotic cell, and cards representing cell structures and biochemical processes involved in protein synthesis.

Coordination of N,O-donor appended Schiff base ligand (H2L1) towards Zinc(II) in presence of pseudohalides: Syntheses, crystal structures, photoluminescence, antimicrobial activities and Hirshfeld surfaces

Science.gov (United States)

Majumdar, Dhrubajyoti; Biswas, Jayanta Kumar; Mondal, Monojit; Surendra Babu, M. S.; Metre, Ramesh K.; Das, Sourav; Bankura, Kalipada; Mishra, Dipankar

2018-03-01

A series of dinuclear Zn(II) complexes [Zn2 (L1) (CH3OH)2(SCN) (OAc)](1), [Zn2 (L1) (CH3OH)2(N3)2](2) and [Zn2 (L1) (Cl)2(CH3OH)]·CH3OH (3) have been synthesized by the reaction of compartmental Schiff base ligand (H2L1) [N,N‧-Bis(3-ethoxysalicylidenimino)-1,3-diaminopropane] with Zn(OAc)2·2H2O in presence of coligand like KSCN, NaN3 and NaCl respectively. X-ray diffraction analysis revealed that all the complexes are neutral and possess a 4-membered Zn2 (μ2-O)2 ring fastened by the unified coordination action of a doubly deprotonated ligand. In addition, solid state structure of the complexes display extensive intermolecular interaction which has been supported theoretically by Hirshfeld surface analysis with 2D Fingerprint plots. The synthesized Zn(II) metal complexes observed enhancement of luminescence emission compared to the parent Schiff base due to emanating ligand based intraligand (π→π∗) fluorescence. Additionally, Zn(II) metal complexes exhibited considerable antimicrobial potency against some important Gram +ve and Gram -ve bacteria.

Deposition of newly synthesized histones: new histones H2A and H2B do not deposit in the same nucleosome with new Histones H3 and H4

International Nuclear Information System (INIS)

Jackson, V.

1987-01-01

The authors have developed procedures to study histone-histone interactions during the deposition of histones in replicating cells. Cells are labeled for 60 min with dense amino acids, and subsequently, the histones within the nucleosomes are cross-linked into an octameric complex with formaldehyde. These complexes are sedimented to equilibrium in density gradients and octamer and dioctamer complexes separated by sodium dodecyl sulfate-polyacrylamide gel electrophoresis. With reversal of the cross-link, the distribution of the individual density-labeled histones in the octamer is determined. Newly synthesized H3 and H4 deposits as a tetramer and are associated with old H2A and H2B. Newly synthesized H2A and H2B deposit as a dimer associated with old H2A, H2B, H3, and H4. The significance of these results with respect to the dynamics of histone interactions in the nucleus is discussed. Control experiments are presented to test for artifactual formation of these complexes during preparative procedures. In addition, reconstitution experiments were performed to demonstrate that the composition of these octameric complexes can be determined from their distribution of density gradients

Optimizing complex scandium-3,3 benzilidene BIS [4-hydroxycoumarin] with 46Sc radiotracer

International Nuclear Information System (INIS)

Khanza Aktari Dewi; Muhamad Basit Febrian; Duyeh Setiawan

2015-01-01

Coumarin, coumarin derivatives and coumarin complex compounds known to possess biological activities such as anticancer and antiviral. The reaction between the active compound coumarin derivatives with radioisotopes Sc-46 is expected to give a complex that will be marked for further investigation of its biological activity in purpose of drug development based on coumarin. This study aims to determine the optimum conditions in the synthesis of its complex compounds as well as the physico chemical characteristics including physical properties and radiochemical purity of the complex. 3.3 benzilidene bis [4-hydroxycoumarin] ligand has successfully synthesized by reacting 4-hydroxycoumarin with benzaldehyde. Complex solids formed instantly when the solution ScCl 3 labeled by Sc-46 with a pH of 5 is reacted with a ligand solution with a pH of 11 with the optimum ratio of Sc: ligand were 1:2 with optimum labeling percentage of 99,75 ± 0,02%. FTIR analysis of complex compounds and ligands show some shift in absorption due to the formation of complex. Melting point of ligand was 234°C whilst complex compound was not yet melted in maximum range of Fischer-Jons instrument at 300°C. The complex was white reddish coloured and well soluble in DMSO. Radiochemical purity of the complex Sc-(3,3 benzilidene bis [4-hydroxycoumarin]) 2 .2H 2 O was 91.22%. Complex compound of coumarin labeled by Sc-46 has been successfully synthesized and characterized with proposed molecular formula of Sc-(3,3 benzilidene bis [4-hydroxycoumarin]) 2 .2H 2 O. (author)

Local Structure in Americium and Californium Hexa-cyanoferrates - Comparison with Their Lanthanide Analogues

International Nuclear Information System (INIS)

Dupouy, G.; Bonhoure, I.; Dumas, Th.; Moisy, Ph.; Petit, S.; Den Auwer, Ch.; Conradson, St.D.; Hennig, Ch.; Scheinost, A.C.; Le Naour, C.; Simoni, E.

2011-01-01

Metal hexa-cyanoferrates are well known molecular solids for a large variety of cations, although very little has been described for actinide adducts. Two new members of actinide(III) hexa-cyanoferrates were synthesized with the cations americium and californium. They were structurally characterized by infrared and X-ray absorption spectroscopy. Combined EXAFS data at the iron K edge and actinide L 3 edge provide evidence for a three-dimensional model for these two new compounds. Structural data in terms of bond lengths were compared to those reported for the parent lanthanide(III) compounds, neodymium and gadolinium hexa-cyanoferrates, respectively: the americium compound with (KNd(III)Fe(II)-Fe-III(CN) 6 .4H 2 O and the californium compound with (KGd(III)Fe(II)(CN) . 3.5H 2 O and (KGd(III)Fe(II)(CN) 6 .3H 2 O. This comparison between actinide and lanthanide homologues has been carried out on the basis of ionic radii considerations. The americium and neodymium environments appear to be very similar and are arranged in a tri-capped trigonal prism polyhedron of coordination number 9 (CN: 9), in which the americium atom is bonded to six nitrogen atoms and to three water molecules. For the californium adduct, a similar comparison and bond length and angle values derived from EXAFS studies suggest that the californium cation sits in a bi-capped trigonal prism (CN: 8) as in (KGd(III)Fe(II)(CN) 6 . 3H 2 O. This arrangement differs from that in the structure of (KGd(III)Fe(II)(CN) 6 .3.5H 2 O, in which the gadolinium atom is surrounded by 9 atoms. This is one of the rare pieces of information revealed by EXAFS spectroscopy for americium and californium in comparison to lanthanide atoms in molecular solid compounds. A discussion on the decrease in bond length and coordination number from americium to californium is also provided, on the basis of crystallographic results reported in the literature for actinide(III) and lanthanide(III) hydrate series. (authors)

A low-spurious fast-hopping MB-OFDM UWB synthesizer

Energy Technology Data Exchange (ETDEWEB)

Chen Danfeng; Li Wei; Li Ning; Ren Junyan, E-mail: w-li@fudan.edu.c [State Key Laboratory of ASIC and System, Fudan University, Shanghai 201203 (China)

2010-06-15

A frequency synthesizer for the ultra-wide band (UWB) group no. 1 is proposed. The synthesizer uses a phase-locked loop (PLL) and single-sideband (SSB) mixers to generate the three center frequencies of the first band group by mixing 4224 MHz with {+-}264 MHz and 792 MHz, respectively. A novel multi-QSSB mixer is designed to combine the function of frequency selection and frequency conversion for low power and high linearity. The synthesizer is fabricated in Jazz 0.18-{mu}m RF CMOS technology. The measured reference spur is as low as -69 dBc and the maximum spur is the LO leakage of -32 dBc. A low phase noise of -110 dBc/Hz - 1 MHz offset and an integrated phase noise of 1.86{sup 0} are achieved. The hopping time between different bands is less than 1.8 ns. The synthesizer consumes 30 mA from a 1.8 V supply. (semiconductor integrated circuits)

A low-spurious fast-hopping MB-OFDM UWB synthesizer

International Nuclear Information System (INIS)

Chen Danfeng; Li Wei; Li Ning; Ren Junyan

2010-01-01

A frequency synthesizer for the ultra-wide band (UWB) group no. 1 is proposed. The synthesizer uses a phase-locked loop (PLL) and single-sideband (SSB) mixers to generate the three center frequencies of the first band group by mixing 4224 MHz with ±264 MHz and 792 MHz, respectively. A novel multi-QSSB mixer is designed to combine the function of frequency selection and frequency conversion for low power and high linearity. The synthesizer is fabricated in Jazz 0.18-μm RF CMOS technology. The measured reference spur is as low as -69 dBc and the maximum spur is the LO leakage of -32 dBc. A low phase noise of -110 dBc/Hz - 1 MHz offset and an integrated phase noise of 1.86 0 are achieved. The hopping time between different bands is less than 1.8 ns. The synthesizer consumes 30 mA from a 1.8 V supply. (semiconductor integrated circuits)

Syntheses, crystal and band structures, and optical properties of a selenidoantimonate and an iron polyselenide

Energy Technology Data Exchange (ETDEWEB)

Liu, Guang-Ning, E-mail: chm_liugn@ujn.edu.cn [Key Laboratory of Chemical Sensing and Analysis in Universities of Shandong, School of Chemistry and Chemical Engineering, University of Jinan, Jinan, Shandong 250022 (China); Zhu, Wen-Juan [Key Laboratory of Chemical Sensing and Analysis in Universities of Shandong, School of Chemistry and Chemical Engineering, University of Jinan, Jinan, Shandong 250022 (China); Zhang, Ming-Jian [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Xu, Bo; Liu, Qi-Sheng; Zhang, Zhen-Wei [Key Laboratory of Chemical Sensing and Analysis in Universities of Shandong, School of Chemistry and Chemical Engineering, University of Jinan, Jinan, Shandong 250022 (China); Li, Cuncheng, E-mail: chm_licc@ujn.edu.cn [Key Laboratory of Chemical Sensing and Analysis in Universities of Shandong, School of Chemistry and Chemical Engineering, University of Jinan, Jinan, Shandong 250022 (China)

2014-10-15

A new selenidoantimonate (CH{sub 3}NH{sub 4})[Mn(phen){sub 2}](SbSe{sub 4})·phen (1, phen=1,10-phenanthroline) and an iron polyselenide [Fe(phen){sub 2}](Se{sub 4}) (2) were obtained under hydro(solvo)thermal conditions. Compound 1 represents the first example of a selenidoantimonate anion as a ligand to a transition-metal π-conjugated ligand complex cation. Compound 2 containing a κ{sup 2}Se{sup 1},Se{sup 4} chelating tetraselenide ligand, represents the only example of a tetraselenide ligand to a Fe complex cation. Compounds 1 and 2 exhibit optical gaps of 1.71 and 1.20 eV, respectively and their thermal stabilities have been investigated by thermogravimetric analyses. The electronic band structure along with the density of states calculated by the DFT method indicate that the optical absorptions mainly originate from the charge transitions from the Se 4p and Mn 3d states to the phen p–π{sup ⁎} orbital for 1 and the Se 4p and Fe 3d states to the phen p–π{sup ⁎} orbital for 2. - Graphical abstract: Two metal–Se complexes, representing the only example of a selenidoantimonate ligand to a TM π-conjugated ligand complex, and a tetraselenide ligand to a Fe complex cation, were synthesized. - Highlights: • The first π-conjugated ligand complex containing selenidoantimonate was isolated. • The first example of a tetraselenide ligand to a Fe complex cation was reported. • We found that phen can adjust the optical band gaps of metal–Se complexes.

Syntheses, crystal and band structures, and optical properties of a selenidoantimonate and an iron polyselenide

International Nuclear Information System (INIS)

Liu, Guang-Ning; Zhu, Wen-Juan; Zhang, Ming-Jian; Xu, Bo; Liu, Qi-Sheng; Zhang, Zhen-Wei; Li, Cuncheng

2014-01-01

A new selenidoantimonate (CH 3 NH 4 )[Mn(phen) 2 ](SbSe 4 )·phen (1, phen=1,10-phenanthroline) and an iron polyselenide [Fe(phen) 2 ](Se 4 ) (2) were obtained under hydro(solvo)thermal conditions. Compound 1 represents the first example of a selenidoantimonate anion as a ligand to a transition-metal π-conjugated ligand complex cation. Compound 2 containing a κ 2 Se 1 ,Se 4 chelating tetraselenide ligand, represents the only example of a tetraselenide ligand to a Fe complex cation. Compounds 1 and 2 exhibit optical gaps of 1.71 and 1.20 eV, respectively and their thermal stabilities have been investigated by thermogravimetric analyses. The electronic band structure along with the density of states calculated by the DFT method indicate that the optical absorptions mainly originate from the charge transitions from the Se 4p and Mn 3d states to the phen p–π ⁎ orbital for 1 and the Se 4p and Fe 3d states to the phen p–π ⁎ orbital for 2. - Graphical abstract: Two metal–Se complexes, representing the only example of a selenidoantimonate ligand to a TM π-conjugated ligand complex, and a tetraselenide ligand to a Fe complex cation, were synthesized. - Highlights: • The first π-conjugated ligand complex containing selenidoantimonate was isolated. • The first example of a tetraselenide ligand to a Fe complex cation was reported. • We found that phen can adjust the optical band gaps of metal–Se complexes

Complex Macromolecular Architectures by Living Cationic Polymerization

KAUST Repository

Alghamdi, Reem D.

2015-05-01

Poly (vinyl ether)-based graft polymers have been synthesized by the combination of living cationic polymerization of vinyl ethers with other living or controlled/ living polymerization techniques (anionic and ATRP). The process involves the synthesis of well-defined homopolymers (PnBVE) and co/terpolymers [PnBVE-b-PCEVE-b-PSiDEGVE (ABC type) and PSiDEGVE-b-PnBVE-b-PSiDEGVE (CAC type)] by sequential living cationic polymerization of n-butyl vinyl ether (nBVE), 2-chloroethyl vinyl ether (CEVE) and tert-butyldimethylsilyl ethylene glycol vinyl ether (SiDEGVE), using mono-functional {[n-butoxyethyl acetate (nBEA)], [1-(2-chloroethoxy) ethyl acetate (CEEA)], [1-(2-(2-(t-butyldimethylsilyloxy)ethoxy) ethoxy) ethyl acetate (SiDEGEA)]} or di-functional [1,4-cyclohexanedimethanol di(1-ethyl acetate) (cHMDEA), (VEMOA)] initiators. The living cationic polymerizations of those monomers were conducted in hexane at -20 0C using Et3Al2Cl3 (catalyst) in the presence of 1 M AcOEt base.[1] The PCEVE segments of the synthesized block terpolymers were then used to react with living macroanions (PS-DPE-Li; poly styrene diphenyl ethylene lithium) to afford graft polymers. The quantitative desilylation of PSiDEGVE segments by n-Bu4N+F- in THF at 0 °C led to graft co- and terpolymers in which the polyalcohol is the outer block. These co-/terpolymers were subsequently subjected to “grafting-from” reactions by atom transfer radical polymerization (ATRP) of styrene to afford more complex macromolecular architectures. The base assisted living cationic polymerization of vinyl ethers were also used to synthesize well-defined α-hydroxyl polyvinylether (PnBVE-OH). The resulting polymers were then modified into an ATRP macro-initiator for the synthesis of well-defined block copolymers (PnBVE-b-PS). Bifunctional PnBVE with terminal malonate groups was also synthesized and used as a precursor for more complex architectures such as H-shaped block copolymer by “grafting-from” or �

Synthesis and characterisation of ruthenium(III) complexes with benzimidazole derivatives

International Nuclear Information System (INIS)

Vyas, P.C.; Kaur, N.; Goel, A.K.; Vyas, S.

1995-01-01

Complexes of ruthenium trichloride with biologically important benzimidazole derivatives, viz., 2-(hydroxy methyl) benzimidazole, 2-(l-hydroxy ethyl) benzimidazole, 2-(mercapto methyl) benzimidazole, 2-(l-mercapto ethyl) benzimidazole, and 2,2'-bis-benzimidazole have been synthesized by reacting the above metal chloride and ligands respectively in 1:3 molar ratio. These complexes are characterised on the basis of elemental analysis, molar conductance data, room temperature, magnetic moment values, electronic spectral and IR spectral studies. (author). 17 refs., 2 tabs

Novel one-pot synthesis of dicarboxylic acids mediated alginate-zirconium biopolymeric complex for defluoridation of water.

Science.gov (United States)

Prabhu, Subbaiah Muthu; Meenakshi, Sankaran

2015-04-20

The present investigation explains the fluoride removal from aqueous solution using alginate-zirconium complex prepared with respective dicarboxylic acids like oxalic acid (Ox), malonic acid (MA) and succinic acid (SA) as a medium. The complexes viz., alginate-oxalic acid-zirconium (Alg-Ox-Zr), alginate-malonic acid-zirconium (Alg-MA-Zr) and alginate-succinic acid-zirconium (Alg-SA-Zr) were synthesized and studied for fluoride removal. The synthesized complexes were characterized by FTIR, XRD, SEM with EDAX and mapping images. The effects of various operating parameters were optimized. The result showed that the maximum removal of fluoride 9653mgF(-)/kg was achieved by Alg-Ox-Zr complex at acidic pH in an ambient atmospheric condition. Equilibrium data of Alg-Ox-Zr complex was fitted well with Freundlich isotherm. The calculated values of thermodynamic parameters indicated that the fluoride adsorption is spontaneous and endothermic in nature. The mechanism of fluoride removal behind Alg-Ox-Zr complex has been proposed in detail. The suitability of the Alg-Ox-Zr complex has been tested with the field sample collected in a nearby fluoride endemic area. Copyright © 2014 Elsevier Ltd. All rights reserved.

Hexanuclear, heterometallic, Ni₃Ln₃ complexes possessing O-capped homo- and heterometallic structural subunits: SMM behavior of the dysprosium analogue.

Science.gov (United States)

Goura, Joydeb; Guillaume, Rogez; Rivière, Eric; Chandrasekhar, Vadapalli

2014-08-04

The reaction of hetero donor chelating mannich base ligand 6,6'-{(2-(dimethylamino)ethylazanediyl)bis(methylene)}bis(2-methoxy-4-methylphenol) with Ni(ClO4)2·6H2O and lanthanide(III) salts [Dy(III) (1); Tb(III) (2); Gd (III) (3); Ho(III) (4); and Er(III) (5)] in the presence of triethylamine and pivalic acid afforded a series of heterometallic hexanuclear Ni(II)-Ln(III) coordination compounds, [Ni3Ln3(μ3-O)(μ3-OH)3(L)3(μ-OOCCMe3)3]·(ClO4)·wCH3CN·xCH2Cl2·yCH3OH·zH2O [for 1, w = 8, x = 3, y = 0, z = 5.5; for 2, w = 0, x = 5, y = 0, z = 6.5; for 3, w = 15, x = 18, y = 3, z = 7.5; for 4, w = 15, x = 20, y = 6, z = 9.5; and for 5, w = 0, x = 3, y = 2, z = 3]. The molecular structure of these complexes reveals the presence of a monocationic hexanuclear derivative containing one perchlorate counteranion. The asymmetric unit of each of the hexanuclear derivatives comprises the dinuclear motif [NiLn(L)(μ3-O)(μ3-OH)(μ-Piv)]. The cation contains three interlinked O-capped clusters: one Ln(III)3O and three Ni(II)Ln(III)2O. Each of the lanthanide centers is eight- coordinated (distorted trigonal-dodecahedron), while the nickel centers are hexacoordinate (distorted octahedral). The study of the magnetic properties of all compounds are reported and suggests single molecule magnet behavior for the Dy(III) derivative (1).

Vibrational imaging of newly synthesized proteins in live cells by stimulated Raman scattering microscopy

Science.gov (United States)

Wei, Lu; Yu, Yong; Shen, Yihui; Wang, Meng C.; Min, Wei

2013-01-01

Synthesis of new proteins, a key step in the central dogma of molecular biology, has been a major biological process by which cells respond rapidly to environmental cues in both physiological and pathological conditions. However, the selective visualization of a newly synthesized proteome in living systems with subcellular resolution has proven to be rather challenging, despite the extensive efforts along the lines of fluorescence staining, autoradiography, and mass spectrometry. Herein, we report an imaging technique to visualize nascent proteins by harnessing the emerging stimulated Raman scattering (SRS) microscopy coupled with metabolic incorporation of deuterium-labeled amino acids. As a first demonstration, we imaged newly synthesized proteins in live mammalian cells with high spatial–temporal resolution without fixation or staining. Subcellular compartments with fast protein turnover in HeLa and HEK293T cells, and newly grown neurites in differentiating neuron-like N2A cells, are clearly identified via this imaging technique. Technically, incorporation of deuterium-labeled amino acids is minimally perturbative to live cells, whereas SRS imaging of exogenous carbon–deuterium bonds (C–D) in the cell-silent Raman region is highly sensitive, specific, and compatible with living systems. Moreover, coupled with label-free SRS imaging of the total proteome, our method can readily generate spatial maps of the quantitative ratio between new and total proteomes. Thus, this technique of nonlinear vibrational imaging of stable isotope incorporation will be a valuable tool to advance our understanding of the complex spatial and temporal dynamics of newly synthesized proteome in vivo. PMID:23798434

Information Retrieval for Ecological Syntheses

Science.gov (United States)

Bayliss, Helen R.; Beyer, Fiona R.

2015-01-01

Research syntheses are increasingly being conducted within the fields of ecology and environmental management. Information retrieval is crucial in any synthesis in identifying data for inclusion whilst potentially reducing biases in the dataset gathered, yet the nature of ecological information provides several challenges when compared with…

Synthesis, spectroscopic, structural and thermal characterizations of vanadyl(IV) adenine complex prospective as antidiabetic drug agent

Science.gov (United States)

El-Megharbel, Samy M.; Hamza, Reham Z.; Refat, Moamen S.

2015-01-01

The vanadyl(IV) adenine complex; [VO(Adn)2]ṡSO4; was synthesized and characterized. The molar conductivity of this complex was measured in DMSO solution that showed an electrolyte nature. Spectroscopic investigation of the green solid complex studied here indicate that the adenine acts as a bidentate ligand, coordinated to vanadyl(IV) ions through the nitrogen atoms N7 and nitrogen atom of amino group. Thus, from the results presented the vanadyl(IV) complex has square pyramid geometry. Further characterizations using thermal analyses and scanning electron techniques was useful. The aim of this paper was to introduce a new drug model for the diabetic complications by synthesized a novel mononuclear vanadyl(IV) adenine complex to mimic insulin action and reducing blood sugar level. The antidiabetic ability of this complex was investigated in STZ-induced diabetic mice. The results suggested that VO(IV)/adenine complex has antidiabetic activity, it improved the lipid profile, it improved liver and kidney functions, also it ameliorated insulin hormone and blood glucose levels. The vanadyl(IV) complex possesses an antioxidant activity and this was clear through studying SOD, CAT, MDA, GSH and methionine synthase. The current results support the therapeutic potentiality of vanadyl(IV)/adenine complex for the management and treatment of diabetes.

Deep embedding convolutional neural network for synthesizing CT image from T1-Weighted MR image.

Science.gov (United States)

Xiang, Lei; Wang, Qian; Nie, Dong; Zhang, Lichi; Jin, Xiyao; Qiao, Yu; Shen, Dinggang

2018-07-01

Recently, more and more attention is drawn to the field of medical image synthesis across modalities. Among them, the synthesis of computed tomography (CT) image from T1-weighted magnetic resonance (MR) image is of great importance, although the mapping between them is highly complex due to large gaps of appearances of the two modalities. In this work, we aim to tackle this MR-to-CT synthesis task by a novel deep embedding convolutional neural network (DECNN). Specifically, we generate the feature maps from MR images, and then transform these feature maps forward through convolutional layers in the network. We can further compute a tentative CT synthesis from the midway of the flow of feature maps, and then embed this tentative CT synthesis result back to the feature maps. This embedding operation results in better feature maps, which are further transformed forward in DECNN. After repeating this embedding procedure for several times in the network, we can eventually synthesize a final CT image in the end of the DECNN. We have validated our proposed method on both brain and prostate imaging datasets, by also comparing with the state-of-the-art methods. Experimental results suggest that our DECNN (with repeated embedding operations) demonstrates its superior performances, in terms of both the perceptive quality of the synthesized CT image and the run-time cost for synthesizing a CT image. Copyright © 2018. Published by Elsevier B.V.

Taxol: A complex diterpenoid natural product with an evolutionarily ...

African Journals Online (AJOL)

In addition to Taxus sp, taxoids are also synthesized by various endophytic fungi, which often live in association with Taxus trees, thus raising questions about the evolutionary origin of this complex diterpenoid pathway. In the future, it may be possible to improve taxoid synthesis through the genetic modification of Taxus cell ...

Photocatalysis of Yttrium Doped BaTiO3 Nanofibres Synthesized by Electrospinning

Directory of Open Access Journals (Sweden)

Zhenjiang Shen

2015-01-01

Full Text Available Yttrium doped barium titanate (BT nanofibres (NFs with significant photocatalytic effect were successfully synthesized by electrospinning. Considering the necessary factors for semiconductor photocatalysts, a well-designed procedure was carried out to produce yttrium doped BT (BYT NFs. In contrast to BYT ceramics powders and BT NFs, BYT NFs with pure perovskite phase showed much enhanced performance of photocatalysis. The surface modification in electrospinning and subsequent annealing, the surface spreading of transition metal yttrium, and the narrowed band gap energy in yttrium doping were all contributed to the final novel photocatalytic effect. This work provides a direct and efficient route to obtain doped NFs, which has a wide range of potential applications in areas based on complex compounds with specific surface and special doping effect.

Fast, High-Precision Optical Polarization Synthesizer for Ultracold-Atom Experiments

Science.gov (United States)

Robens, Carsten; Brakhane, Stefan; Alt, Wolfgang; Meschede, Dieter; Zopes, Jonathan; Alberti, Andrea

2018-03-01

We present a technique for the precision synthesis of arbitrary polarization states of light with a high modulation bandwidth. Our approach consists of superimposing two laser light fields with the same wavelength, but with opposite circular polarizations, where the phase and the amplitude of each light field are individually controlled. We find that the polarization-synthesized beam reaches a degree of polarization of 99.99%, which is mainly limited by static spatial variations of the polarization state over the beam profile. We also find that the depolarization caused by temporal fluctuations of the polarization state is about 2 orders of magnitude smaller. In a recent work, Robens et al. [Low-Entropy States of Neutral Atoms in Polarization-Synthesized Optical Lattices, Phys. Rev. Lett. 118, 065302 (2017), 10.1103/PhysRevLett.118.065302] demonstrated an application of the polarization synthesizer to create two independently controllable optical lattices which trap atoms depending on their internal spin state. We use ultracold atoms in polarization-synthesized optical lattices to give an independent, in situ demonstration of the performance of the polarization synthesizer.

nanoparticles synthesized by citrate precursor m

African Journals Online (AJOL)

user

(M=Co, Cu) nanoparticles synthesized by citrate precursor method ... The structural characterization was carried out using an X-ray Diffractometer (Rikagu Miniflex, Japan) ..... His current area of interest includes magnetic nanomaterials.

Synthesis and characterization of U(VI) and Th(IV) complexes with o-vanillin-p-phenylenediamine

International Nuclear Information System (INIS)

Bi Caifeng; Fan Yuhua

2001-01-01

Two new solid complexes of uranyl nitrate and thorium nitrate with bis-Schiff base o-vanillin-p-phenylenediamine (L) have been synthesized and characterized by elemental analysis, IR, UV, DTA-TG and molar conductance. The compositions of the complexes are confirmed to be [UO 2 LNO 3 ]NO 3 and [ThL(NO 3 ) 2 ](NO 3 ) 2 . Some properties of the complexes are studied

Synthesis and characterization of Th(IV) and U(VI) complexes with o-vanillin-p-phenylenediamine

International Nuclear Information System (INIS)

Bi Caifeng; Fan Yuhua; Sun Guoxin; Chang Jun

2000-01-01

Two new solid complexes, [ThL(NO 3 ) 2 ](NO 3 ) 2 , [UO 2 L(NO 3 )]NO 3 (L = o-vanillin-p-phenylenediamine) have been synthesized and characterized by elemental analyses, DTA-TG, IR spectra, UV spectra and molar conductance. Possible structures of the two complexes are proposed. (author)

Spectrochemical study on different ligand neodymium complexes

International Nuclear Information System (INIS)

Khomenko, V.S.; Lozinskij, M.O.; Fialkov, Yu.A.; Krasovskaya, L.I.; Rasshinina, T.A.; AN Ukrainskoj SSR, Kiev. Inst. Organicheskoj Khimii)

1986-01-01

A series of new adducts of neodymium complexes with 1, 1, 1, 5, 5, 5-hexafluoropentadione - 2, 4 and 2-heptafluoropropoxy-1, 1, 1, 2-tetrafluoro-5-phenylpentadione-3, 5: Nd(HFPTFPhPD) 3 x2H 2 O, Nd(HFPTFPhPD) 3 xDipy, Nd(HFPTFPhPD) 3 xPhen, Nd(HFPTFPhPD) 3 xDphen, Nd(HFA) 3 x2H 2 O, Nd(HFA) 3 xDipy, Nd(HFA) 3 xPhen, Nd(HFA) 3 xDphen, have been synthesized. Ways of their fragmentation under electron impact are established. Bond strength of additional ligands with central atom in the complexes studied is evaluated. Data on decomposition mechanisms of bicharged ions have been obtained for the first time. Addition of bis-heterocycles to neodymium three-ligand complexes changes the properties of the complexes - their thermal stability and photochemical stability increase, in certain cases their volatility increases

Synthesis and characterization of an iron complex bearing a cyclic tetra-N-heterocyclic carbene ligand: An artifical heme analogue?

KAUST Repository

Anneser, Markus R.

2015-04-20

An iron(II) complex with a cyclic tetradentate ligand containing four N-heterocyclic carbenes was synthesized and characterized by means of NMR and IR spectroscopies, as well as by single-crystal X-ray structure analysis. The iron center exhibits an octahedral coordination geometry with two acetonitrile ligands in axial positions, showing structural analogies with porphyrine-ligated iron complexes. The acetonitrile ligands can readily be substituted by other ligands, for instance, dimethyl sulfoxide, carbon monoxide, and nitric oxide. Cyclic voltammetry was used to examine the electronic properties of the synthesized compounds. © 2015 American Chemical Society.

Using Tc-Re chemical analogy to synthesize and identify new 99mTc complexes

International Nuclear Information System (INIS)

Gambino, D.; Kremer, C.; Cartesio, S.; Leon, A.; Kremer, E.

1989-01-01

The strong chemical resemblance between Tc and Re is applied to design and evaluate experiments with 99m Tc complexes. A combination of spectrophotometric and electrophoretic techniques allows to propose the formula [TcO 2 (amine) 2 ] + for compounds prepared by reduction of 99m TcO 4 - with Zn (solid phase) in presence of several (bidentate) amines. (author) 10 refs.; 2 figs.; 4 tabs

Self-assembly of proglycinin and hybrid proglycinin synthesized in vitro from cDNA

Science.gov (United States)

Dickinson, Craig D.; Floener, Liliane A.; Lilley, Glenn G.; Nielsen, Niels C.

1987-01-01

An in vitro system was developed that results in the self-assembly of subunit precursors into complexes that resemble those found naturally in the endoplasmic reticulum. Subunits of glycinin, the predominant seed protein of soybeans, were synthesized from modified cDNAs using a combination of the SP6 transcription and the rabbit reticulocyte translation systems. Subunits produced from plasmid constructions that encoded either Gy4 or Gy5 gene products, but modified such that their signal sequences were absent, self-assembled into trimers equivalent in size to those precursors found in the endoplasmic reticulum. In contrast, proteins synthesized in vitro from Gy4 constructs failed to self-assemble when the signal sequence was left intact (e.g., preproglycinin) or when the coding sequence was modified to remove 27 amino acids from an internal hydrophobic region, which is highly conserved among the glycinin subunits. Various hybrid subunits were also produced by trading portions of Gy4 and Gy5 cDNAs and all self-assembled in our system. The in vitro assembly system provides an opportunity to study the self-assembly of precursors and to probe for regions important for assembly. It will also be helpful in attempts to engineer beneficial nutritional changes into this important food protein. Images PMID:16593868

Proteins synthesized in tobacco mosaic virus infected protoplasts

International Nuclear Information System (INIS)

Huber, R.

1979-01-01

The author deals with research on the multiplication of tobacco mosaic virus (TMV) in leaf cell protoplasts. An attempt is made to answer three questions: (1) Which proteins are synthesized in TMV infected protoplasts as a result of TMV multiplication. (2) Which of the synthesized proteins are made under the direction of the TMV genome and, if any, which of the proteins are host specific. (3) In which functions are these proteins involved. (Auth.)

Some organoperoxo complexes of antimony, niobium and tantalum and their oxidation properties

International Nuclear Information System (INIS)

Tarafder, M.T.H.

1999-05-01

Several novel organoperoxo complexes of Nb(V), Ta(V) and Sb(V) have been synthesized and characterized. The complexes have the compositions [M(O 2 ) 2 L Cl] and [M(O 2 ) 2 L'] [L = monodentate and bidentate, neutral ligand; L' = bidentate, uninegative ligand]. These complexes are very reactive to both organic and inorganic substrates. Niobium and tantalum complexes were found to oxidize phosphines and arsines to their oxides. These also oxidize olefins to epoxides under stoichiometric conditions while under catalytic conditions, ring opening of the epoxides occur producing α-hydroxyketone when the substrate is trans-stilbene. The antimony complexes are decidedly inert towards oxidation. (author)

Novel bi-metallic uranyl complexes - Redox chemistry in aqueous solutions

International Nuclear Information System (INIS)

Yardeni, A.; Mizrahi, E.; Maimon, I.; Zilbermann, G.; Meyerstein, D.; Zehavi-cohen, A.Z.

2014-01-01

The synthesis of organic ligands which can accommodate two uranium atoms at different oxidation states, mixed valency being then achieved by redox chemistry at room temperature is definitely a challenge in coordination chemistry. The following complexes were synthesized and characterized by elemental analysis, NMR, MS, IR and UV-vis

Well-Defined Copper(I) Fluoroalkoxide Complexes for Trifluoroethoxylation of Aryl and Heteroaryl Bromides

KAUST Repository

Huang, Ronglu

2015-03-17

© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. Copper(I) fluoroalkoxide complexes bearing dinitrogen ligands were synthesized and the structure and reactivity of the complexes toward trifluoroethoxylation, pentafluoropropoxylation, and tetrafluoropropoxylation of aryl and heteroaryl bromides were investigated. Efficiency drive: A series of copper(I) fluoroalkoxide complexes bearing N,N ligands have been prepared and structurally characterized. These well-defined complexes serve as efficient reagents for the fluoroalkoxylation of aryl and heteroaryl bromides to produce a wide range of trifluoroethyl, pentafluoropropyl, and tetrafluoropropyl (hetero)aryl ethers in good to excellent yields.

Characterization of Microstructure and Performance of YBa2Cu3O7−x Films Synthesized Through Sol–Gel Aqueous Precursors with DEA/TEA Addition

DEFF Research Database (Denmark)

Tang, Xiao; He, Dong; Zhao, Yichun

2013-01-01

YBa2Cu3O7−x (YBCO) superconducting thin films are synthesized through non-fluorine sol–gel aqueous processes. Diethanolamine (DEA) and triethonalamine (TEA), which have similar molecular structures but different complexation abilities and molecular weights, are separately used as chelating agents...

A series of luminescent Re(I) complexes with electron-donor/acceptor moieties: Synthesis, characterization, and photoluminescence

International Nuclear Information System (INIS)

Ge Hu; Qing She; Lei Guo

2012-01-01

In this paper, we synthesize three Re(I) complexes of Re(CO) 3 (PPO)Br, Re(CO) 3 (PTO)Br, and Re(CO) 3 (PBI)Br, where PPO=2-phenyl-5-(pyridin-2-yl)-1,3,4-oxadiazole, PTO=2-(pyridin-2-yl)-5-p-tolyl-1,3,4-oxadiazole, PBI=2-(pyridin-2-yl)-1H-benzo[d]imidazole. Their single crystals and photophysical properties are measured and discussed in detail. The correlation between ligand structure and corresponding PL characteristics of Re(I) complex has been investigated. It is found that a ligand with strong electron-donor can efficiently increase both absorption and emissive energy of Re(I) complex. In addition, electron-rich ligand can increase the electron density of the complex and thus enhance the oscillator strength of electronic transition, improving the photoluminescence performance. - Highlights: ► Three novel phosphorescent Re(I) complexes are synthesized. ► Molecular structures, photophysical, and electronic properties are studied. ► Strong electron-donor can increase emissive energy. ► Electron-rich ligand can enhance the oscillator strength of electronic transition.

Structural and photoluminescence properties of aligned Sb-doped ZnO nanocolumns synthesized by the hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Fang Xuan [School of Science, Changchun University of Science and Technology, 7089-WeiXing Road, Changchun, 130022 (China); Key Laboratory of Excited State Processes, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, 16 East Nan-Hu Road, Open Economic Zone Changchun, 130033 (China); Li Jinhua [School of Science, Changchun University of Science and Technology, 7089-WeiXing Road, Changchun, 130022 (China); Zhao Dongxu, E-mail: dxzhao2000@yahoo.com.c [Key Laboratory of Excited State Processes, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, 16 East Nan-Hu Road, Open Economic Zone Changchun, 130033 (China); Li Binghui; Zhang Zhenzhong; Shen Dezhen [Key Laboratory of Excited State Processes, Changchun Institute of Optics, Fine Mechanics and Physics, Chinese Academy of Sciences, 16 East Nan-Hu Road, Open Economic Zone Changchun, 130033 (China); Wang Xiaohua; Wei Zhipeng [School of Science, Changchun University of Science and Technology, 7089-WeiXing Road, Changchun, 130022 (China)

2010-08-02

Aligned Sb-doped ZnO nanocolumns were synthesized by a simple hydrothermal method. Based on the analyses of the X-ray diffraction and photoluminescence result, it could be confirmed that the Sb has successfully doped in the ZnO crystal lattices to form an accepter energy level. At 85 K, the recombination of the acceptor-bound exciton was predominant in PL spectrum, which was attributed to the transition of the (Sb{sub Zn}-2V{sub Zn}) complex bound exciton. The acceptor binding energy had been calculated to be 123 meV.

Structural and photoluminescence properties of aligned Sb-doped ZnO nanocolumns synthesized by the hydrothermal method

International Nuclear Information System (INIS)

Fang Xuan; Li Jinhua; Zhao Dongxu; Li Binghui; Zhang Zhenzhong; Shen Dezhen; Wang Xiaohua; Wei Zhipeng

2010-01-01

Aligned Sb-doped ZnO nanocolumns were synthesized by a simple hydrothermal method. Based on the analyses of the X-ray diffraction and photoluminescence result, it could be confirmed that the Sb has successfully doped in the ZnO crystal lattices to form an accepter energy level. At 85 K, the recombination of the acceptor-bound exciton was predominant in PL spectrum, which was attributed to the transition of the (Sb Zn -2V Zn ) complex bound exciton. The acceptor binding energy had been calculated to be 123 meV.

SYNTH: A spectrum synthesizer

International Nuclear Information System (INIS)

Hensley, W.K.; McKinnon, A.D.; Miley, H.S.; Panisko, M.E.; Savard, R.M.

1993-10-01

A computer code has been written at the Pacific Northwest Laboratory (PNL) to synthesize the results of typical gamma ray spectroscopy experiments. The code, dubbed SYNTH, allows a user to specify physical characteristics of a gamma ray source, the quantity of the nuclides producing the radiation, the source-to-detector distance and the presence of absorbers, the type and size of the detector, and the electronic set up used to gather the data. In the process of specifying the parameters needed to synthesize a spectrum, several interesting intermediate results are produced, including a photopeak transmission function versus energy, a detector efficiency curve, and a weighted list of gamma and x rays produced from a set of nuclides. All of these intermediate results are available for graphical inspection and for printing. SYNTH runs on personal computers. It is menu driven and can be customized to user specifications. SYNTH contains robust support for coaxial germanium detectors and some support for sodium iodide detectors. SYNTH is not a finished product. A number of additional developments are planned. However, the existing code has been compared carefully to spectra obtained from National Institute for Standards and Technology (NIST) certified standards with very favorable results. Examples of the use of SYNTH and several spectral results are presented

Symmetric bi-pyridyl banana-shaped molecule and its intermolecular hydrogen bonding liquid-crystalline complexes

Science.gov (United States)

Sui, Dan; Hou, Qiufei; Chai, Jia; Ye, Ling; Zhao, Liyan; Li, Min; Jiang, Shimei

2008-11-01

A new symmetric bi-pyridyl banana-shaped molecule 1,3-phenylene diisonicotinate (PDI) was designed and synthesized. Its molecular structure was confirmed by FTIR, Elemental analysis and 1H NMR. X-ray crystallographic study reveals that there is an angle of approximate 118° among the centroids of the three rings (pyridyl-phenyl-pyridyl) in each PDI molecule indicating a desired banana shape. In addition, a series of liquid crystal complexes nBA:PDI:nBA induced by intermolecular hydrogen bonding between PDI (proton acceptor) and 4-alkoxybenzoic acids (nBA, proton donor) were synthesized and characterized. The mesomorphism properties and optical textures of the complex of nBA:PDI:nBA were investigated by differential scanning calorimetry, polarizing optical microscope and X-ray diffraction.

Partial strands synthesizing leads to inevitable aborting and complicated products in consecutive polymerase chain reactions (PCRs)

Institute of Scientific and Technical Information of China (English)

2007-01-01

Various abnormal phenomena have been observed during PCR so far. The present study performed a series of consecutive PCRs (including many rounds of re-amplification continuously) and found that the abortion of re-amplification was inevitable as long as a variety of complicated product appeared. The aborting stages varied, according to the lengths of targets. Longer targets reached the abortion earlier than the shorter ones, marked by appearance of the complex that was immobile in electropho-resis. Denatured gel-electrophoresis revealed that the complex was mainly made up of shorter or partially synthesized strands, together with small amounts of full-length ones. Able to be digested by S1 nuclease but unable by restriction endonucleases (REs), the complex was proved to consist of both single regions and double-helix regions that kept the complex stable thermodynamically. Simulations gave evidence that partial strands, even at lower concentration, could disturb re-amplification effec- tively and lead to the abortion of re-amplifications finally. It was pointed out that the partial strands formed chiefly via polymerase’s infidelity, and hence the solution to lighten the abnormality was also proposed.

Synthesis, structural characterization and cytotoxic activity of two new organoruthenium(II complexes

Directory of Open Access Journals (Sweden)

SANJA GRGURIC-SIPKA

2008-06-01

Full Text Available Two new p-cymene ruthenium(II complexes containing as additional ligands N-methylpiperazine ([(η6-p-cymeneRuCl2(CH3NH(CH24NH]PF6, complex 1 or vitamin K3-thiosemicarbazone ([(η6-p-cymeneRuCl2(K3tsc], complex 2 were synthesized starting from [(η6-p-cymene2RuCl2]2 and the corresponding ligand. The complexes were characterized by elemental analysis, IR, electronic absorption and NMR spectroscopy. The X-ray crystal structure determination of complex 1 revealed “piano-stool” geometry. The differences in the cytotoxic activity of the two complexes are discussed in terms of the ligand present.

Synthesis, Physical Characterization and Biological Activity of Some Schiff Base Complexes

Directory of Open Access Journals (Sweden)

R. Rajavel

2008-01-01

Full Text Available Structural modification of organic molecule has considerable biological relevance. Further, coordination of a biomolecules to the metal ions significantly alters the effectiveness of the biomolecules. In view of the antimicrobial activity ligand [bis-(2-aminobenzaldehyde] malonoyl dihydrazone], metal complexes with Cu(II, Ni(II, Zn(II and oxovanadium(IV have been synthesized and found to be potential antimicrobial agents. An attempt is also made to correlate the biological activities with geometry of the complexes. The complexes have been characterized by elemental analysis, molar conductance, spectra and cyclicvoltammetric measurements. The structural assessment of the complexes has been carried out based on electronic, infrared and molar conductivity values.

Synthesis of Fe–C{sub 60} complex by ion irradiation

Energy Technology Data Exchange (ETDEWEB)

Minezaki, Hidekazu, E-mail: dn1000012@toyo.jp [Graduate School of Engineering, Toyo University, 2100 Kujirai, Kawagoe, Saitama 350-8585 (Japan); Oshima, Kosuke [Graduate School of Engineering, Toyo University, 2100 Kujirai, Kawagoe, Saitama 350-8585 (Japan); Uchida, Takashi; Mizuki, Toru [Bio-Nano Electronics Research Centre, Toyo University, 2100 Kujirai, Kawagoe, Saitama 350-8585 (Japan); Racz, Richard [Institute of Nuclear Research (ATOMKI), H-4026, Debrecen, Bem tér 18/C (Hungary); Muramatsu, Masayuki [National Institute of Radiological Sciences (NIRS), 4-9-1 Anagawa, Inage-ku, Chiba-shi, Chiba 263-8555 (Japan); Asaji, Toyohisa [Oshima National College of Maritime Technology, 1091-1 Komatsu Suou Oshima City, Oshima, Yamaguchi 742-2193 (Japan); Kitagawa, Atsushi [National Institute of Radiological Sciences (NIRS), 4-9-1 Anagawa, Inage-ku, Chiba-shi, Chiba 263-8555 (Japan); Kato, Yushi [Graduate School of Engineering, Osaka University, 2-1 Yamada-oka, Suita-shi, Osaka 565-0871 (Japan); Biri, Sandor [Institute of Nuclear Research (ATOMKI), H-4026, Debrecen, Bem tér 18/C (Hungary); Yoshida, Yoshikazu [Graduate School of Engineering, Toyo University, 2100 Kujirai, Kawagoe, Saitama 350-8585 (Japan); Bio-Nano Electronics Research Centre, Toyo University, 2100 Kujirai, Kawagoe, Saitama 350-8585 (Japan)

2013-09-01

Highlights: •The Fe{sup +} beam was irradiated to the C{sub 60} thin films. •The Fe{sup +}-irradiated C{sub 60} thin films were analyzed by LDI-TOF-MS and by HPLC. •The peak with mass/charge of 776 was observed in the Fe{sup +}-irradiated C{sub 60} thin film. •We could synthesize the Fe–C{sub 60} complex as a new material. -- Abstract: In order to synthesize the Fe@C{sub 60} complex, iron ion beam irradiated to C{sub 60} thin films. The energy of the irradiated iron ions was controlled from 50 eV to 250 eV. The dose of that was controlled from 6.67 × 10{sup 12} to 6.67 × 10{sup 14} ions/cm{sup 2}. By the analysis of the surface of the iron ion irradiated C{sub 60} thin films using laser desorption/ionization time-of-flight mass spectrometry, we could confirm the peak with mass/charge of 776. The mass/charge of 776 corresponds to Fe + C{sub 60}. We obtained the maximum intensity of the peak with mass/charge of 776 under the irradiation iron ion energy and the dose were 50 eV and 3.30 × 10{sup 13} ions/cm{sup 2}, respectively. Then, the separation of the material with mass of 776 was performed by using high performance liquid chromatography. We could separate the Fe + C{sub 60} from the iron ion irradiated C{sub 60} thin film. As a result, we could synthesize the Fe + C{sub 60} complex as a new material.

Forward osmosis for oily wastewater reclamation: Multi-charged oxalic acid complexes as draw solutes

KAUST Repository

Ge, Qingchun

2017-06-11

Forward osmosis (FO) has demonstrated its merits in hybrid FO seawater desalination. However, FO may have a potential for other applications if suitable draw solutes are available. In this study, a series of novel draw solutes based on oxalic acid (OA)-transitional metal complexes are presented. Influential factors of FO performance have been systematically investigated by varying the transitional metals, cations of the complex draw solutes as well as the experimental conditions. Compared to NaCl and other recently synthesized draw solutes, the OA complexes show superior FO performance in terms of high water fluxes up to 27.5 and 89.1 LMH under the respective FO and PRO (pressure retarded osmosis) modes, both with negligible reverse solute fluxes. The features of octahedral geometry, abundant hydrophilic groups and ionic species are crucial for the OA complexes as appropriate draw solutes with satisfactory FO performance. Among the synthesized OA complexes, the ammonium salt of chromic complex (NH4-Cr-OA) outperforms others due to the presence of more ionic species in its complex system. NH4-Cr-OA also performs better than the typical NaCl draw solute in FO oily wastewater treatment with higher water recovery and negligible reverse fluxes. Dilute solutions of OA complexes have been reconcentrated through membrane distillation (MD) and reused to new round of FO processes. The OA complexes have demonstrated their suitability and superiority as a novel class of draw solutes for the FO process in this study.

General Syntheses of Nanotubes Induced by Block Copolymer Self-Assembly

DEFF Research Database (Denmark)

Zhao, Jianming; Huang, Wei; Si, Pengchao

2018-01-01

Amphiphilic block copolymer templating strategies are extensively used for syntheses of mesoporous materials. However, monodisperse tubular nanostructures are limited. Here, a general method is developed to synthesize monodisperse nanotubes with narrow diameter distribution induced by self...

A mononuclear zinc(II) complex with piroxicam: Crystal structure, DNA- and BSA-binding studies; in vitro cell cytotoxicity and molecular modeling of oxicam complexes

Science.gov (United States)

Jannesari, Zahra; Hadadzadeh, Hassan; Amirghofran, Zahra; Simpson, Jim; Khayamian, Taghi; Maleki, Batool

2015-02-01

A new mononuclear Zn(II) complex, trans-[Zn(Pir)2(DMSO)2], where Pir- is 4-hydroxy-2-methyl-N-2-pyridyl-2H-1,2-benzothiazine-3-carboxamide-1,1-dioxide (piroxicam), has been synthesized and characterized. The crystal structure of the complex was obtained by the single crystal X-ray diffraction technique. The interaction of the complex with DNA and BSA was investigated. The complex interacts with FS-DNA by two binding modes, viz., electrostatic and groove binding (major and minor). The microenvironment and the secondary structure of BSA are changed in the presence of the complex. The anticancer effects of the seven complexes of oxicam family were also determined on the human K562 cell lines and the results showed reasonable cytotoxicities. The interactions of the oxicam complexes with BSA and DNA were modeled by molecular docking and molecular dynamic simulation methods.

Comparison on Bactericidal and Cytotoxic Effect of Silver Nanoparticles Synthesized by Different Methods

Science.gov (United States)

Mala, R.; Celsia, A. S. Ruby; Malathi Devi, S.; Geerthika, S.

2017-08-01

Biologically synthesized silver nanoparticle are biocompatible for medical applications. The present work is aimed to synthesize silver nanoparticle using the fruit pulp of Tamarindusindica and to evaluate its antibacterial and anticancer activity against lung cancercell lines. Antibacterial activity was assessed by well diffusion method. Cytotoxicity was evaluated using MTT assay. GC-MS of fruit pulp extract showed the presence of levoglucosenone, n-hexadecanoic acid, 9,12-octadecadienoic acid etc. Antioxidant activity of the fruit pulp was determined by DPPH assay, hydrogen peroxide scavenging assay and lipid peroxidation. The size of biologically synthesized silver nanoparticle varied from 50 nm to 76 nm. It was 59 nm to 98 nm for chemically synthesized silver nanoparticle. Biologically synthesized silver nanoparticle showed 26 mm inhibition zone against E. coli and chemically synthesized silver nanoparticle showed 20 mm. Antioxidant activity of fruit extract by DPPH showed 84 % reduction. The IC 50 of biologically synthesized silver nanoparticle against lung cancer cell lines was 48 µg/ml. It was 95 µg/ml for chemically synthesized silver nanoparticle. The increased activity of biologically synthesized silver nanoparticle was due to its smaller size, stability and the bioactive compounds capping the silver nanoparticle extracted from the fruit extract.

Rare-earth organic frameworks involving three types of architecture tuned by the lanthanide contraction effect: hydrothermal syntheses, structures and luminescence.

Science.gov (United States)

Deng, Zhao-Peng; Kang, Wei; Huo, Li-Hua; Zhao, Hui; Gao, Shan

2010-07-21

The first example of rare-earth organic frameworks with 3-aminopyrazine-2-carboxylic acid (Hapca) was synthesized under hydrothermal conditions and characterized by elemental analysis, IR, PL, TG, powder and single-crystal X-ray diffraction. These ten complexes exhibit three different structure types with decreasing lanthanide radii: [La(apca)(3)](n) () for type I, {[Ln(apca)(ox)(H(2)O)(2)].H(2)O}(n) (Ln = Pr (2), Nd (3), ox = oxalate) for type II, and [Ln(2)(apca)(4)(OH)(2)(H(2)O)(2)](n) (Ln = Sm (4), Eu (5), Gd (6), Tb (7), Dy (8), Er (9), Y (10)) for type III. The structure of type I consists of 1D "snowflake" chains along a-axis, which are further interconnected by hydrogen bonds to produce a 3D sra net topology containing infinite (-C-O-La-)(n) rod-shaped SBU. Type II has 2D Ln-apca-ox 4(4)-net, in which a planar udud water tetramers (H(2)O)(4) are formed by coordinated and free water molecules. Type III also comprises of 2D 4(4)-layer network constructed from Ln-apca-OH. The structure diversity is mainly caused by the variation of coordinated ligand and lanthanide contraction effect. Remarkably, the oxalate in type II was in situ synthesized from 3-aminopyrazine-2-carboxylic acid through an oxidation-hydrolysis reaction. The luminescent investigations reveal that complex exhibits strong blue emission and complex exhibits characteristic luminescence of Eu(3+).

Evaluation of Biological Activities of Chemically Synthesized Silver Nanoparticles

International Nuclear Information System (INIS)

Mostafa, A. A.; Solkamy, E.N.; Sayed, Sh. R. M.; Khan, M.; Shaik, M.R.; Al-Warthan, A.; Adil, S.F.

2015-01-01

Silver nanoparticles were synthesized by the earlier reported methods. The synthesized nanoparticles were characterized using ultraviolet-visible spectrophotometry (UV/Vis), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDX), and X-ray powder diffraction (XRD). The synthesized materials were also evaluated for their antibacterial activity against Gram positive and Gram negative bacterial strains. TEM micrograph showed the spherical morphology of AgNPs with size range of 40-60 nm. The synthesized nanoparticles showed a strong antimicrobial activity and their effect depends upon bacterial strain as AgNPs exhibited greater inhibition zone for Pseudomonas aeruginosa (19.1 mm) followed by Staphylococcus aureus (14.8?mm) and S. pyogenes (13.6 mm) while the least activity was observed for Salmonella typhi (12.5 mm) at concentration of 5 μg/disc. The minimum inhibitory concentration (MIC) of AgNPs against S. aureus was 2.5 μg/disc and less than 2.5 μg/disc for P. aeruginosa. These results suggested that AgNPs can be used as an effective antiseptic agent for infectious control in medical field.

Thermochemical properties of rare earth complexes with salicylic acid

International Nuclear Information System (INIS)

Yang Xuwu; Sun Wujuan; Ke Congyu; Zhang Hangguo; Wang Xiaoyan; Gao Shengli

2007-01-01

Fourteen rare earth complexes with salicylic acid RE(HSal) 3 .nH 2 O (HSal = C 7 H 5 O 3 ; RE = La-Sm, n = 2; RE = Eu-Lu, n = 1) were synthesized and characterized by elemental analysis, and their thermal decomposition mechanism were studied with TG-DTG technology. The constant-volume combustion energies of complexes, Δ c U, were determined by a precise rotating-bomb calorimeter at 298.15 K. Their standard molar enthalpies of combustion, Δ c H m 0 , and standard molar enthalpies of formation, Δ f H m o , were calculated

Ruthenium (II) complexes of thiosemicarbazone: Synthesis, biosensor applications and evaluation as antimicrobial agents

International Nuclear Information System (INIS)

Yildirim, Hatice; Guler, Emine; Yavuz, Murat; Ozturk, Nurdan; Kose Yaman, Pelin; Subasi, Elif; Sahin, Elif; Timur, Suna

2014-01-01

A conformationally rigid half-sandwich organoruthenium (II) complex [(η 6 -p-cymene)RuClTSC N–S ]Cl, (1) and carbonyl complex [Ru(CO)Cl(PPh 3 ) 2 TSC N–S ] (2) have been synthesized from the reaction of [{(η 6 -p-cymene)RuCl} 2 (μ-Cl) 2 ] and [Ru(H)(Cl)(CO)(PPh 3 ) 3 ] with thiophene-2-carboxaldehyde thiosemicarbazon (TSC) respectively and both novel ruthenium (II) complexes have been characterized by elemental analysis, FT-IR and NMR spectroscopy. The peripheral TSC in the complexes acts as an electrochemical coupling unit providing the ability to carry out electrochemical deposition (ED) and to form an electro-deposited film on a graphite electrode surface. The biosensing applicability of complexes 1 and 2 was investigated by using glucose oxidase (GOx) as a model enzyme. Electrochemical measurements at − 0.9 V versus Ag/AgCl electrode by following the ED Ru(II) reduction/oxidation due to from the enzyme activity, in the presence of glucose substrate. The designed biosensor showed a very good linearity for 0.01–0.5 mM glucose. The in vitro antimicrobial activities of complexes 1 and 2 were also investigated against nine bacterial strains and one fungus by the disc diffusion test method. No activity was observed against the Gram-negative strains and fungus, whereas complex 1 showed moderate antibacterial activities against Gram-positive bacterial strains. - Highlights: • Novel Ru (II) thiosemicarbazone complexes were synthesized and characterized. • Electrochemical depositions were performed. • Rigid half-sandwich Ru (II) complex showed enhanced antibacterial activity

Syntheses and studies of organosilicon compounds

Energy Technology Data Exchange (ETDEWEB)

Xie, Ren [Iowa State Univ., Ames, IA (United States)

1999-02-12

The syntheses of polycarbosilanes and polysilanes as silicon carbide ceramic precursors have been active research areas in the Barton Research Group. In this thesis, the work is focused on the preparation of polycarbosilanes and polysilanes as stoichiometric silicon carbide precursor polymers. The syntheses of the precursor polymers are discussed and the conversions of these precursors to silicon carbide via pyrolysis are reported. The XRD pattern and elemental analyses of the resulting silicon carbide ceramics are presented. Silicon monoxide is an important intermediate in the production of silicon metal. The existence of silicon monoxide in gap phase has been widely accepted. In the second part of this thesis, the generation of gaseous silicon monoxide in four different reactors and the reactions of gaseous silicon monoxide towards organic compounds are discussed.

An AIE-active boron-difluoride complex: multi-stimuli-responsive fluorescence and application in data security protection.

Science.gov (United States)

Zhu, Xiaolin; Liu, Rui; Li, Yuhao; Huang, Hai; Wang, Qiang; Wang, Danfeng; Zhu, Xuan; Liu, Shishen; Zhu, Hongjun

2014-11-04

A novel AIE-active boron-difluoride complex (PTZ) was synthesized which exhibits multi-stimuli responsive characteristics. Its colours and emissions can be switched by mechanical grinding, organic solvent vapours and acid/base vapours. This complex can be utilized in data encryption and decryption based on the protonation-deprotonation effect.

Synthesis, characterization and biocidal activities of heterobimetallic complexes having tin(IV) as a padlock

Science.gov (United States)

Husain, Ahmad; Nami, Shahab A. A.; Siddiqi, K. S.

2010-04-01

A mononuclear precursor complex, [(CH 3) 2Sn(tpdtc)] and several of its heterobimetallic derivatives of the type, [(CH 3) 2Sn(tpdtc)]MCl 2 have been synthesized by the simple addition reaction of transition metal chlorides, MCl 2· nH 2O where tpdtc = tetraethylenepentamine bis(dithiocarbamate) anion, M = Fe(II), Co(II), Ni(II), Cu(II) and Zn(II). The synthesized complexes have been systematically characterized by the physicochemical and spectroscopic techniques. A square-pyramidal geometry has been proposed for all the transition metal atoms with chloride ions occupying the axial while the three nitrogen atoms occupying the equatorial positions. A symmetrical bidentate coordination has been observed for the dithiocarbamato moiety leading to the formation of 18 member cavity. The thermal studies reveal that the mononuclear complex decomposes in three stages while its heterobimetallic analog exhibits a simple two-stage profile. The conductivity measurement data (1 mmol solution) implies a non-electrolytic behavior for all the complexes as evident by their low conductivity values obtained at room temperature. The heterobimetallic complexes have also been tested against the bacterial ( Escherichia coli and Pseudomonas aeruginosa) and antifungal strains ( Aspergillus niger and Fusarium oxysporum). All the complexes were found to be active against the test organisms and maximum activity was found for [(CH 3) 2Sn(tpdtc)]CuCl 2 complex.

Bioinorganic Relevance of Some Cobalt(II Complexes with Thiophene-2-glyoxal Derived Schiff Bases

Directory of Open Access Journals (Sweden)

Prashant Singh

2009-01-01

Full Text Available Complexes of Co(II with two new Schiff bases TEAB [2-hydroxy-4-{[2-oxo-2-(thiophen-2-ylethylidene]amino}benzoic acid] and TEPC [N-[2-oxo-2-(thiophen-2-ylethylidene]pyridine-3-carboxamide] have been synthesized and characterized with the help of elemental analysis, magnetic, mass, 1H-NMR, 13C-NMR, IR and electronic spectral data. IR spectra manifest the coordination of the ligand to the metal ion through the carbonyl oxygen, azomethine nitrogen and thienyl sulphur atoms. With the help of electronic spectral data various ligand field parameters were also calculated. All these studies reveal the distorted octahedral Co(II complexes. Synthesized compounds have also been screened against some micro organisms viz, Escherichia coli, Proteus vulgaris, Aspergillus niger and Aspergillus flavus with the help of ‘filter paper disc’ technique. It has been observed that the antimicrobial activities of metal complexes are higher than that of the free ligand.

Synthesis, magnetic and spectral studies of lanthanide(III) chloride complexes of hydrazones of isonicotinic acid hydrazide

International Nuclear Information System (INIS)

Agarwal, R.K.; Agarwal, Himanshu; Prasad, Ram

1996-01-01

The synthesis, magnetic and spectral properties of trivalent lanthanide chlorides with N-isonicotinamidobenzalaldimine (INH-BENZ), N-isonicotinamidoanisalaldimine (INH-ANSL) and N-isonicotinamido-p-dimethylaminobenzalaldimine (INH-PDAB) are described. 13 refs., 2 tabs

Gadolinium DTPA-monoamide complexes incorporated into mixed micelles as possible MRI contrast agents

OpenAIRE

Parac-Vogt, Tatjana; Kimpe, Kristof; Laurent, Sophie; Pierart, Corinne; Vander Elst, Luce; Muller, Robert N.; Binnemans, Koen

2004-01-01

Four monoamide derivatives of Gd-DTPA with alkyl chains consisting of 12, 14, 16, or 18 carbon atoms were synthesized. The gadolinium(III) complexes with chain lengths of 14, 16 or 18 carbon atoms were efficiently incorporated into mixed micelles whereas the complex with a chain length of 12 carbon atoms was not incorporated into a micellar structure. The size distribution of the micelles was measured by photon correlation spectroscopy. The mean sizes of the micelles for all the complexes lay...

Biomedical applications of green synthesized Nobel metal nanoparticles.

Science.gov (United States)

Khan, Zia Ul Haq; Khan, Amjad; Chen, Yongmei; Shah, Noor S; Muhammad, Nawshad; Khan, Arif Ullah; Tahir, Kamran; Khan, Faheem Ullah; Murtaza, Behzad; Hassan, Sadaf Ul; Qaisrani, Saeed Ahmad; Wan, Pingyu

2017-08-01

Synthesis of Nobel metal nanoparticles, play a key role in the field of medicine. Plants contain a substantial number of organic constituents, like phenolic compounds and various types of glycosides that help in synthesis of metal nanoparticles. Synthesis of metal nanoparticles by green method is one of the best and environment friendly methods. The major significance of the green synthesis is lack of toxic by-products produced during metal nanoparticle synthesis. The nanoparticles, synthesized by green method show various significant biological activities. Most of the research articles report the synthesized nanoparticles to be active against gram positive and gram negative bacteria. Some of these bacteria include Escherichia coli, Bacillus subtilis, Klebsiella pneumonia and Pseudomonas fluorescens. The synthesized nanoparticles also show significant antifungal activity against Trichophyton simii, Trichophyton mentagrophytes and Trichophyton rubrum as well as different types of cancer cells such as breast cancer cell line. They also exhibit significant antioxidant activity. The activities of these Nobel metal nano-particles mainly depend on the size and shape. The particles of small size with large surface area show good activity in the field of medicine. The synthesized nanoparticles are also active against leishmanial diseases. This research article explores in detail the green synthesis of the nanoparticles and their uses thereof. Copyright © 2017 Elsevier B.V. All rights reserved.

Antibacterial activity of silver nanoparticles synthesized from serine

Energy Technology Data Exchange (ETDEWEB)

Jayaprakash, N. [Catalysis and Nanomaterials Research Laboratory, Department of Chemistry, Loyola College, Chennai 600 034 (India); SRM Valliammai Engineering College, Department of Chemistry, Chennai 603 203 (India); Judith Vijaya, J., E-mail: jjvijayaloyola@yahoo.co.in [Catalysis and Nanomaterials Research Laboratory, Department of Chemistry, Loyola College, Chennai 600 034 (India); John Kennedy, L. [Materials Division, School of Advanced Sciences, VIT University, Chennai Campus, Chennai 600 048 (India); Priadharsini, K.; Palani, P. [Department of Center for Advanced Study in Botany, University of Madras, Guindy Campus, Chennai 600 025 (India)

2015-04-01

Silver nanoparticles (Ag NPs) were synthesized by a simple microwave irradiation method using polyvinyl pyrrolidone (PVP) as a capping agent and serine as a reducing agent. UV–Visible spectra were used to confirm the formation of Ag NPs by observing the surface plasmon resonance (SPR) band at 443 nm. The emission spectrum of Ag NPs showed an emission band at 484 nm. In the presence of microwave radiation, serine acts as a reducing agent, which was confirmed by Fourier transformed infrared (FT-IR) spectrum. High-resolution transmission electron microscopy (HR-TEM) and high-resolution scanning electron microscopy (HR-SEM) were used to investigate the morphology of the synthesized sample. These images showed the sphere-like morphology. The elemental composition of the sample was determined by the energy dispersive X-ray analysis (EDX). Selected area electron diffraction (SAED) was used to find the crystalline nature of the Ag NPs. The electrochemical behavior of the synthesized Ag NPs was analyzed by the cyclic voltammetry (CV). Antibacterial experiments showed that the prepared Ag NPs showed relatively similar antibacterial activities, when compared with AgNO{sub 3} against Gram-positive and Gram-negative bacteria. - Highlights: • Microwave irradiation method is used to synthesize silver nanoparticles. • Highly stable silver nanoparticles are produced from serine. • A detailed study of antibacterial activities is discussed. • Formation mechanism of silver microspheres has been proposed.

Ferromagnetic dinuclear mixed-valence Mn(II)/Mn(III) complexes: building blocks for the higher nuclearity complexes. structure, magnetic properties, and density functional theory calculations.

Science.gov (United States)

Hänninen, Mikko M; Välivaara, Juha; Mota, Antonio J; Colacio, Enrique; Lloret, Francesc; Sillanpää, Reijo

2013-02-18

A series of six mixed-valence Mn(II)/Mn(III) dinuclear complexes were synthesized and characterized by X-ray diffraction. The reactivity of the complexes was surveyed, and structures of three additional trinuclear mixed-valence Mn(III)/Mn(II)/Mn(III) species were resolved. The magnetic properties of the complexes were studied in detail both experimentally and theoretically. All dinuclear complexes show ferromagnetic intramolecular interactions, which were justified on the basis of the electronic structures of the Mn(II) and Mn(III) ions. The large Mn(II)-O-Mn(III) bond angle and small distortion of the Mn(II) cation from the ideal square pyramidal geometry were shown to enhance the ferromagnetic interactions since these geometrical conditions seem to favor the orthogonal arrangement of the magnetic orbitals.

A series of copper complexes with carbazole and oxadiazole moieties: Synthesis, characterization and luminescence performance

Energy Technology Data Exchange (ETDEWEB)

Bai Weiyang, E-mail: baiwy02@163.com [College of Chemistry and Chemical Engineering, Chongqing University of Technology, Chongqing 400054 (China); Sun Li [Graduate University of Chinese Academy of Sciences, Beijing 100049 (China)

2012-10-15

In this paper, various moieties of ethyl, carbazole and oxadiazole are attached to 2-thiazol-4-yl-1H-benzoimidazole to form a series of diamine ligands. Their corresponding Cu(I) complexes are also synthesized using bis(2-(diphenylphosphanyl)phenyl) ether as the auxiliary ligand. Crystal structures, thermal property, electronic nature and luminescence property of these Cu(I) complexes are discussed in detail. These Cu(I) complexes are found to be efficient green-emitting ones in solutions and the emissive parameters are improved largely by the incorporation of substituent moieties. Detailed analysis suggests that the effective suppression of solvent-induced exciplex quenching is responsible for this phenomenon. On the other hand, the introduction of substituent moieties exerts no obvious influence on molecular structure, thermal stability and emitting-energy of the Cu(I) complexes, owing to their absence from inner coordination sphere. - Highlights: Black-Right-Pointing-Pointer Diamine ligands with various moieties and Cu(I) complexes are synthesized. Black-Right-Pointing-Pointer Crystal structures and photophysical property are discussed in detail. Black-Right-Pointing-Pointer The incorporation of substituent moieties improves luminescence performance. Black-Right-Pointing-Pointer Solvent-induced exciplex quenching is suppressed by substituent moieties.

Collaborative Management of Risks and Complexity in Banking Systems

Directory of Open Access Journals (Sweden)

Ion IVAN

2012-01-01

Full Text Available This paper describes types of risks encountered in banking systems and ways to prevent and eliminate them. Banking systems are presented in order to have a view on banking activities and processes that generates risks. The risks in banking processes are analyzed and the collaborative character of risk management is highlighted. A way to control the risk in banking systems through information security is described. Risks arise from system complexity, thus evaluation and comparison of different configurations are bases for improvements. The Halstead relative complexity function synthesizes system complexity from the point of view of the size of the variables analyzed and the heterogeneity between the variables. Section four was realized by Catalin SBORA.

Cyclometalated Iridium(III) Complexes Containing 4,4'-π-Conjugated 2,2'-Bipyridine Derivatives as the Ancillary Ligands: Synthesis, Photophysics, and Computational Studies.

Science.gov (United States)

Sarma, Monima; Chatterjee, Tanmay; Bodapati, Ramakrishna; Krishnakanth, Katturi Naga; Hamad, Syed; Rao, S Venugopal; Das, Samar K

2016-04-04

This article demonstrates a series of cyclometalated Ir(III) complexes of the type [Ir(III)(C^N)2(N^N)](PF6), where C^N is 2-phenylpyridine, and N^N corresponds to the 4,4'-π-conjugated 2,2'-bipyridine ancillary ligands. All these compounds were synthesized through splitting of the binuclear dichloro-bridged complex precursor, [Ir(C^N)2(μ-Cl)]2, with the appropriate bipyridine ligands followed by the anion exchange reaction. The linear and nonlinear absorption properties of the synthesized complexes were investigated. The absorption spectra of all the title complexes exhibit a broad structureless feature in the spectral region of 350-700 nm with two bands being well-resolved in most of the cases. The structures of all the compounds were modeled in dichloromethane using the density functional theory (DFT) algorithm. The nature of electronic transitions was further comprehended on the basis of time-dependent DFT analysis, which indicates that the origins of various bands are primarily due to intraligand charge transfer transitions along with mixed-metal and ligand-centered transitions. The synthesized compounds are found to be nonemissive at room temperature because of probable nonradiative deactivation pathways of the T1 state that compete with the radiative (phosphorescence) decay modes. However, the frozen solutions of compounds Ir(MS 3) and Ir(MS 5) phosphoresce at the near-IR region, the other complexes remaining nonemissive up to 800 nm wavelength window. The two-photon absorption studies on the synthesized complexes reveal that values of the absorption cross-section are quite notable and lie in the range of 300-1000 GM in the picosecond case and 45-186 GM in the femtosecond case.

Synthesis and structure determination of a stable organometallic uranium(V) imine complex and its isolobal anionic U(IV)-ate complex

Energy Technology Data Exchange (ETDEWEB)

Sharma, M.; Botoshanskii, M.; Eisen, M.S. [Schulich Faculty of Chemistry, and Institute of Catalysis Science and Technology, Technion Israel Institute of Technology, Haifa (Israel); Bannenberg, Th.; Tamm, M. [Institut fur Anorganische und Analytische Chemie, Technische Universitat Braunschweig (Germany)

2010-06-15

The reaction of one equivalent of Cp*{sub 2}UCl{sub 2} with 2-(trimethylsilyl-imino)-1,3-di-tert-butyl-imidazoline in boiling toluene afforded a one electron oxidation of the uranium metal and the opening of the N-heterocyclic ring, resulting in the formation of an organometallic uranium(V) imine complex. This complex crystallized with one molecule of toluene in the unit cell, and its solid-state structure was determined by X-ray diffraction analysis. When the same reaction was performed in perdeuterated toluene, a myriad of organometallic complexes were obtained, however, when equimolar amounts of water were used in toluene, the same complex was obtained, and its solid state characterization shows two independent molecules in the unit cell with an additional water molecule. For comparison of the geometric parameters, the corresponding isolobal anionic uranium(IV) complex [Cp*{sub 2}UCl{sub 3}]{sup -} was synthesized by the reaction of Cp*{sub 2}UCl{sub 2} with 1,3-di-tert-butyl-imidazolium chloride, and the resulting U(IV)-ate complex was characterized by X-ray diffraction analysis. (authors)

Souper: A Synthesizing Superoptimizer

OpenAIRE

Sasnauskas, Raimondas; Chen, Yang; Collingbourne, Peter; Ketema, Jeroen; Lup, Gratian; Taneja, Jubi; Regehr, John

2017-01-01

If we can automatically derive compiler optimizations, we might be able to sidestep some of the substantial engineering challenges involved in creating and maintaining a high-quality compiler. We developed Souper, a synthesizing superoptimizer, to see how far these ideas might be pushed in the context of LLVM. Along the way, we discovered that Souper's intermediate representation was sufficiently similar to the one in Microsoft Visual C++ that we applied Souper to that compiler as well. Shipp...

Syntheses, crystal structures, and magnetic properties of four new cyano-bridged bimetallic complexes based on the mer-[Fe(III)(qcq)(CN)3]- building block.

Science.gov (United States)

Shen, Xiaoping; Zhou, Hongbo; Yan, Jiahao; Li, Yanfeng; Zhou, Hu

2014-01-06

Four new cyano-bridged bimetallic complexes, [{Mn(III)(salen)}2{Fe(III)(qcq)(CN)3}2]n·3nCH3CN·nH2O (1) [salen = N,N'-ethylenebis(salicylideneiminato) dianion; qcq(-) = 8-(2-quinoline-2-carboxamido)quinoline anion], [{Mn(III)(salpn)}2{Fe(III)(qcq)(CN)3}2]n·4nH2O (2) [salpn = N,N'-1,2-propylenebis(salicylideneiminato)dianion], [{Mn(II)(bipy)(CH3OH)}{Fe(III)(qcq)(CN)3}2]2·2H2O·2CH3OH (3) (bipy = 2,2'-bipyridine), and [{Mn(II)(phen)2}{Fe(III)(qcq)(CN)3}2]·CH3CN·2H2O (4) (phen = 1,10-phenanthroline) have been synthesized and characterized both structurally and magnetically. The structures of 1 and 2 are both unique 1-D linear branch chains with additional structural units of {Mn(III)(salen/salpn)}{Fe(III)(qcq)(CN)3} dangling on the sides. In contrast, 3 and 4 are cyano-bridged bimetallic hexanuclear and trinuclear clusters, respectively. The intermolecular short contacts such as π-π interactions and hydrogen bonds extend 1-4 into high dimensional supermolecular networks. Magnetic investigation reveals the dominant intramolecular antiferromagnetic interactions in 1, 3, and 4, while ferromagnetic and antiferromagnetic interactions coexist in 2. Alternating current measurement at low temperature indicates the existence of slow magnetic relaxation in 1 and 2, which should be due to the single ion anisotropy of Mn(III).

Phthalocyaninato complexes of thorium, protactinium and uranium

International Nuclear Information System (INIS)

Beck, O.F.

1985-01-01

For the preparation of Bis(phthalocyaninato)-actinoid(IV) complexes, AnPc 2 , a new optimizing synthesis procedure was developed, with which it was possible to prepare spectrally pure, that is, H 2 Pc-free, ThPc 2 , UPc 2 and the isostructurally similar 231 PaPc 2 .PaPc 2 . This was verified with the help of electron spectra, which were compared to preparations which were synthesized in another manner. The corresponding perfluorinated compounds were also produced for thorium and uranium by use of tetrafluorophthalic acid nitrile instead of phthalic acid nitrile as initial product. Electron and infrared spectra show the typical bands of the non-substituted complexes. By the attempt to produce a mono(phthalocyaninato)-thorium complex with the use of ThI 4 as initial material a pyridine-extracted pure ThPcI 2 (py) 2 was obtained with a typical mono(phthalocyaninato) complex electron spectrum, an extremely moisture sensitive compound which in water or acids decomposes and produces H 2 Pc. (orig./RB) [de

Synthesis of several tetraaza macrocyclic amine ligands and the biodistribution of their Tc-complexes

International Nuclear Information System (INIS)

Ketring, A.R.

1982-01-01

Several macrocyclic tetraaza ligands were synthesized and their /sup 99m/Tc-complexes prepared. The biological distribution of these complexes was examined to determine their possible utility as radiodiagnostic agents. The simplest of the macrocyclic tetraaza ligands studied, cyclam, forms a very stable cationic complex with Tc when pertechnetate is reduced with stannous ion in an aqueous solution of the ligand. When injected intravenously into mice Tc-cyclam was excreted predominantly by the urinary system. Derivatives of cyclam which were synthesized contained aromatic or aliphatic substituents and formed more lipophilic complexes with Tc. The complexes were formed in high yield as determined by paper chromatography, thin layer chromatography, electrophoresis and/or high performance liquid chromatography. Relative lipophilicities were determined for the complexes by octanol-to-water extractions. Animal studies using mice indicated there was an inverse relationship between the octanol-to-water extraction ratio and urinary excretion. Two of the complexes having relatively high octanol-to-water extraction ratios were significantly excreted by the hepatobiliary system with localization in the gall bladder. The complex having the highest octanol-to-water ratio was not excreted significantly by the hepatobiliary system, but cleared very slowly from the blood and localized in the liver, lungs, spleen and to some extent the heart. Derivatization of cyclam can be performed without greatly reducing its ability to complex Tc but greatly influencing the biological distribution of its Tc complex. This indicates that there is a potential for preparing radiodiagnostic agents using macrocyclic tetraaza ligands

Ruthenium Complexes as NO Donors for Vascular Relaxation Induction

Directory of Open Access Journals (Sweden)

Renata Galvão de Lima

2014-07-01

Full Text Available Nitric oxide (NO donors are substances that can release NO. Vascular relaxation induction is among the several functions of NO, and the administration of NO donors is a pharmacological alternative to treat hypertension. This review will focus on the physicochemical description of ruthenium-derived NO donor complexes that release NO via reduction and light stimulation. In particular, we will discuss the complexes synthesized by our research group over the last ten years, and we will focus on the vasodilation and arterial pressure control elicited by these complexes. Soluble guanylyl cyclase (sGC and potassium channels are the main targets of the NO species released from the inorganic compounds. We will consider the importance of the chemical structure of the ruthenium complexes and their vascular effects.

Rhenium carbene complexes and their applications; Rhenium-Carben-Komplexe und ihre Anwendungen

Energy Technology Data Exchange (ETDEWEB)

Hille, Claudia Heidi

2016-01-25

New pharmaceutically suitable metal complexes play an important role in the development of diagnostic and therapeutic agents for cancer treatment. One option concerning new radiopharmaceuticals, is the application of the rhenium isotopes {sup 186}Re and {sup 188}Re. Therefore, water soluble but at the same time stable complexes, which can be synthesized straightforward, are required. In this thesis, several synthetic pathways to such rhenium complexes bearing Nheterocyclic carbenes are presented and applicability tests of literature known complexes conducted. The selected target structures based on monocarbenes turned out to be inappropriate for use in radiopharmaceutical applications, due to their long reaction times and purification issues. Additionally, sterical and electronical effects of the carbene ligands concerning complex formation have been investigated. Possibilities of functionalization at different positions on the heterocycle as well as hydrophilic wingtips - to achieve a better stability in an aqueous media - have been examined to gain information about chemical and physical properties of the resulting complexes. Furthermore, experiments regarding the coordination of various biscarbene ligands, which provides besides the stable chelatisation additionally the possibility of varying the linking bridge, to rhenium(I/V) precursors, have been performed. Dioxo-bis-(1,1{sup '}-methylene-bis(3,3{sup '}-diisopropylimidazolium-2-ylidene)) rhenium(V )-hexafluorophosphate was synthesized via a transmetalation reaction of the corresponding silver carbene with ReOCl{sub 3}(PPh{sub 3}){sub 2} and silver hexafluorophosphate. This complex provided the basis for the first radiolabeled {sup 188}Rhenium NHC complex later on. An enhancement of the kinetic and thermodynamic stability of potential rhenium biscarbene complexes based on modifications concerning the length and character of the bridging moiety between the chelating NHC rings as well as the nature of

A low-power CMOS frequency synthesizer for GPS receivers

International Nuclear Information System (INIS)

Yu Yunfeng; Xiao Shimao; Zhuang Haixiao; Ma Chengyan; Ye Tianchun; Yue Jianlian

2010-01-01

A low-power frequency synthesizer for GPS/Galileo L1/E1 band receivers implemented in a 0.18 μm CMOS process is introduced. By adding clock-controlled transistors at latch outputs to reduce the time constant at sensing time, the working frequency of the high-speed source-coupled logic prescaler supplying quadrature local oscillator signals has been increased, compared with traditional prescalers. Measurement results show that this synthesizer achieves an in-band phase noise of -87 dBc/Hz at 15 kHz offset, with spurs less than -65 dBc. The whole synthesizer consumes 6 mA in the case of a 1.8 V supply, and its core area is 0.6 mm 2 . (semiconductor integrated circuits)

Synthese en chemotherapeutisch onderzoek van sulfanilamidopyrimidinen

NARCIS (Netherlands)

Grevenstuk, Anton Bernard

1942-01-01

In order to investigate the influence of substitution in the pyrimidine nucleous on the activity of the three isomeric sulfanilamidopyrimidines (2, 5 and 6), a number of substituted sulfanilamidopyrimidines were synthesized and tested on chemotherapeutic activity. ... Zie: Summary

Synthesis and studies on Cu(II), Co(II), Ni(II) complexes of Knoevenagel β-diketone ligands

Science.gov (United States)

Sumathi, S.; Tharmaraj, P.; Sheela, C. D.; Anitha, C.

2012-11-01

Transition metal complexes of various acetylacetone based ligands of the type ML [where M = Cu(II), Ni(II), Co(II); L = 3-(aryl)-pentane-2,4-dione] have been synthesized. The structural features have been derived from their elemental analysis, magnetic susceptibility, molar conductance, IR, UV-Vis, 1H NMR, Mass and ESR spectral studies. Conductivity measurements reveal that all the complexes are non-electrolytic in nature. Spectroscopic and other analytical data of the complexes suggest octahedral geometry for other metal(II) complexes. The redox behavior of the copper(II) complexes have been studied by cyclic voltammetry. The free ligands and their metal complexes have been screened for their in vitro biological activities against the bacteria Pseudomonas aeruginosa, Escherichia coli and Staphylococcus aureus as well as the fungus Candida albicans by well diffusion method. The zone of inhibition value indicates that the most of the metal(II) complexes are found to possess increased activities compared to those of the free ligands. All synthesized compounds may serve as potential photoactive materials as indicated from their characteristic fluorescence properties. The second harmonic generation (SHG) efficiency of the ligands (L1-L3) was found to be considerable effect than that of urea and KDP (potassium dihydrogen phosphate).

Synthesis and Characterization of Chromium (III) Complexes with L-Glutamic Acid, Glycine and LCysteine

OpenAIRE

Kun Sri Budiasih; Chairil Anwar; Sri Juari Santosa; Hilda Ismail

2013-01-01

Some Chromium (III) complexes were synthesized with three amino acids: L Glutamic Acid, Glycine, and L-cysteine as the ligands, in order to provide a new supplement containing Cr(III) for patients with type 2 diabetes mellitus. The complexes have been prepared by refluxing a mixture of Chromium(III) chloride in aqueous solution with L-glutamic acid, Glycine, and L-cysteine after pH adjustment by sodium hydroxide. These complexes were characterized by Infrared and Uv-Vis s...

Promotion of mitochondrial membrane complex assembly by a proteolytically inactive yeast Lon

NARCIS (Netherlands)

Rep, M; van Dijl, J M; Suda, K; Schatz, G; Grivell, L A; Suzuki, C K

1996-01-01

Afg3p and Rca1p are adenosine triphosphate (ATP)-dependent metalloproteases in yeast mitochondria. Cells lacking both proteins exhibit defects in respiration-dependent growth, degradation of mitochondrially synthesized proteins, and assembly of inner-membrane complexes. Defects in growth and protein

Covalently {beta}-cyclodextrin modified single-walled carbon nanotubes: a novel artificial receptor synthesized by 'click' chemistry

Energy Technology Data Exchange (ETDEWEB)

Guo Zhen; Liang Li [Nankai University, State Key Laboratory and Institute of Elemento-Organic Chemistry (China); Liang Jiajie; Ma Yanfeng; Yang Xiaoying [Nankai University, Center for Nanoscale Science and Technology and Institute of Polymer Chemistry, College of Chemistry (China); Ren Dongmei [Nankai University, State Key Laboratory and Institute of Elemento-Organic Chemistry (China); Chen Yongsheng [Nankai University, Center for Nanoscale Science and Technology and Institute of Polymer Chemistry, College of Chemistry (China); Zheng Jianyu, E-mail: jyzheng@nankai.edu.c [Nankai University, State Key Laboratory and Institute of Elemento-Organic Chemistry (China)

2008-08-15

Novel {beta}-cyclodextrin covalently modified single-walled carbon nanotubes have been synthesized via a 'click' coupling reaction. The product was fully characterized with Raman, FTIR, XRD, UV-Vis-NIR spectra as well as TEM and TGA measurements. The effective functionalization via 'click' coupling has set up a facile and versatile route for modular preparation of SWNTs based functional materials. The inclusion complexation behavior of this artificial receptor with quinine has been investigated in aqueous solution by fluorescence spectroscopy.

Synthesis, EPR, Electronic and Magnetic Studies on Cobalt (II) Complexes of Semicarbazone and Thiosemicarbazone

International Nuclear Information System (INIS)

Chandra, S.; Gupta, L.K.; Sharma, K.K.

2005-01-01

Cobalt (II) complexes having the general composition Co(L2) X2 [where Lisopropyl methyl ketone semicarbazone (LLA), isopropyl methyl ketone thiosemicarbazone (LLB), 4-aminoacetophenone semicarbazone (LLC) and4-aminoacetophenone thiosemicarbazone (LLD) and X=Cl] have been synthesized. All the Co(II) complexes reported here have been characterized by elemental analyses, magnetic moments, IR, electronic and EPR spectral studies. All the complexes were found to have magnetic moments corresponding to three unpaired electrons. The possible geometries of the complexes were assigned on the basis of electronic infrared and EPR spectral studies. (author) = = = = = = = = = = = = = = =

SYNTH: A spectrum synthesizer

International Nuclear Information System (INIS)

Hensley, W.K.; McKinnon, A.D.; Miley, H.S.; Panisko, M.E.; Savard, R.M.

1994-07-01

A computer code has been written at the Pacific Northwest Laboratory (PNL) to synthesize the results of typical gamma-ray spectroscopy experiments. The code, dubbed SYNTH, allows a use r to specify physical characteristics of a gamma-ray source, the quantity of the nuclides producing the radiation, the source-to-detector distance and the type and thickness of absorbers, the size and composition of the detector (Ge or NaI), and the electronic set up used to gather the data. In the process of specifying the parameters needed to synthesize a spectrum, several interesting intermediate results are produced, including a photopeak transmission function vs energy, a detector efficiency curve, and a weighted list of gamma and x rays produced from a set of nuclides. All of these intermediate results are available for graphical inspection and for printing. SYNTH runs on personal computers. It is menu driven and can be customized to user specifications. SYNTH contains robust support for coaxial germanium detectors and some support for sodium iodide detectors. SYNTH is not a finished product. A number of additional developments are planned. However, the existing code has been compared carefully to spectra obtained from National Institute for Standards and Technology (NIST) certified standards with very favorable results. Examples of the use of SYNTH and several spectral results will be presented

Photoluminescence of Alq3 - and Tb-activated aluminium-tris(8-hydroxyquinoline) complex for blue chip-excited OLEDs.

Science.gov (United States)

Yawalkar, P W; Dhoble, S J; Thejo Kalyani, N; Atram, R G; Kokode, N S

2013-01-01

The tris(8-hydroxyquinoline)-aluminium complex is the most important and widely studied as electron transporting and green light emitting material. Alq(3) and Tb(x) Al((1-x)) q(3) have been synthesized (where x = 0.1, 0.3, 0.5, 0.7 and 0.9) and blended films of Alq(3) and Tb(x) Al((1-x)) q(3) with PMMA and PS at different percentage weight (wt%) concentrations (e.g., 0.1, 1, 5, 10, 25 and 50 wt%) have been prepared. The synthesized materials and their blended thin films have been characterized by a photoluminescence (PL) technique; the synthesis and PL characterization are reported in this paper. The synthesized metal complex shows bright emission of green light with blue light excitation (440 nm) and the prepared Tb(x) Al((1-x)) q(3) phosphor may be applicable in blue chip-excited OLEDs for the newly developed wallpaper lighting technology. Copyright © 2012 John Wiley & Sons, Ltd.

Synthesis and physicochemical study of rare earth complexes with o-hydroxyphenoxymethylphosphonic acid

International Nuclear Information System (INIS)

Alibaeva, Z.M.; Snezhko, N.I.; Pechurova, N.I.; Martynenko, L.I.; Alekseeva, N.A.; Bovin, A.N.

1987-01-01

Rare earth complexes with o-hydroxyphenoxymethylphosphonic acid (C 7 H 9 PO 5 , N 2 L) of the HMl 2 xnH 2 O composition are synthesized. The compounds separated are studied by IR spectroscopy, X-ray phase and elementary analysis methods. The data obtained permit to suppose on the polymer structure of rare earth complexes, except HLaL 2 x2H 2 O which is evidently of the island structure

A fractional-N frequency synthesizer for wireless sensor network nodes

International Nuclear Information System (INIS)

Ma Xiao; Du Zhankun; Liu Chang; Liu Ke; Yan Yuepeng; Ye Tianchun

2014-01-01

This paper presents a fractional-N frequency synthesizer for wireless sensor network (WSN) nodes. The proposed frequency synthesizer adopts a phase locked loop (PLL) based structure, which employs an LC voltage-controlled oscillator (VCO) with small VCO gain (K VCO ) and frequency step (f step ) variations, a charge pump (CP) with current changing in proportion with the division ratio and a 20-bit ΔΣ modulator, etc. To realize constant K VCO and f step , a novel capacitor sub-bands grouping method is proposed. The VCO sub-groups' sizes are arranged according to the maximal allowed K VCO variation of the system. Besides, a current mode logic divide-by-2 circuit with inside-loop buffers ensures the synthesizer generates I/Q quadrature signals robustly. This synthesizer is implemented in a 0.13 μm CMOS process. Measurement results show that the frequency synthesizer has a frequency span from 2.07 to 3.11 GHz and the typical phase noise is −86.34 dBc/Hz at 100 kHz offset and −114.17 dBc/Hz at 1 MHz offset with a loop bandwidth of about 200 kHz, which meet the WSN nodes' requirements. (semiconductor integrated circuits)

Characterization and optical properties of pole-like nano-CeO{sub 2} synthesized by a facile hydrothermal method

Energy Technology Data Exchange (ETDEWEB)

Wang, Leini [School of Physics and Materials Science, Anhui University, Feixi Road, Hefei 230039 (China); Meng, Fanming, E-mail: mrmeng@ahu.edu.cn [School of Physics and Materials Science, Anhui University, Feixi Road, Hefei 230039 (China); Key Laboratory of Materials Modification by Laser, Ion and Electron Beams (Dalian University of Technology), Ministry of Education, Dalian 116024 (China); Li, Kangkang [Lab of SoC, Department of Microelectronics, Peking University, Beijing 100871 (China); Lu, Fei [Baotou Research Institute of Rare Earths, Baotou 014030 (China)

2013-12-01

CeO{sub 2} nanopoles have been successfully synthesized by a hydrothermal method using CeC{sub l3}·7H{sub 2}O as cerium source, NaOH as mineralizer, and ethylenediamine as complexant. The pole-like nano-CeO{sub 2} was examined by XRD, TEM, XPS, UV–vis, PL, and Raman scattering. The results show that the crystallinity of the nanopoles is not so good, and the main valence of cerium is +4. The estimated direct band gaps are 3.014, 3.099, 2.931, and 2.927 eV for the samples synthesized within 2, 18, 50, and 100 h, respectively. These band gaps are smaller than bulk CeO{sub 2}, oxygen vacancies and Ce{sup 3+} ions result in an effective red shifting of the band gap. The visible luminescence exhibits similar emission peaks of room temperature photoluminescence and the emission intensity increases with the increase of concentration of oxygen vacancies and Ce{sup 3+} ions.

Rational assembly of Pb(II)/Cd(II)/Mn(II) coordination polymers based on flexible V-shaped dicarboxylate ligand: Syntheses, helical structures and properties

Energy Technology Data Exchange (ETDEWEB)

Yang, Gao-Shan [School of Environment and Chemical Engineering, Nanchang Hangkong University, Nanchang 330063 (China); Liu, Chong-Bo, E-mail: cbliu@nchu.edu.cn [School of Environment and Chemical Engineering, Nanchang Hangkong University, Nanchang 330063 (China); School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlanta, GA 30332 (United States); Liu, Hong [School of Environment and Chemical Engineering, Nanchang Hangkong University, Nanchang 330063 (China); Robbins, Julianne; Zhang, Z. John [School of Chemistry and Biochemistry, Georgia Institute of Technology, Atlanta, GA 30332 (United States); Yin, Hong-Shan [School of Environment and Chemical Engineering, Nanchang Hangkong University, Nanchang 330063 (China); Wen, Hui-Liang [State Key Laboratory of Food Science and Technology, Nanchang University, Nanchang 330047 (China); Wang, Yu-Hua [School of Environment and Chemical Engineering, Nanchang Hangkong University, Nanchang 330063 (China)

2015-05-15

Six new coordination polymers, namely, [Pb(L)(H{sub 2}O)] (1), [Pb(L)(phen)] (2), [Pb{sub 2}(L){sub 2}(4,4′-bipy){sub 0.5}] (3), [Cd(L)(phen)] (4), [Cd(L)(4,4′-bipy)]·H{sub 2}O (5) and [Mn(L)(4,4′-bipy)]·H{sub 2}O (6) have been synthesized by the hydrothermal reaction of 2,2′-[hexafluoroisopropylidenebis(p-phenyleneoxy)]diacetic acid (H{sub 2}L) with Pb(II)/Cd(II)/Mn(II) in the presence of ancillary ligands 4,4′-bipyridine (4,4′-bipy) or 1,10-phenanthroline (phen). Complexes 1 and 4–6 exhibit 2-D structures, and complexes 2–3 display 3-D frameworks, of which L{sup 2−} ligands join metal ions to single-stranded helical chains of 1, 3–6 and double-stranded helical chains of 2. Complexes 2 and 3 also contain double-stranded Metal–O helices. Topology analysis reveals that complexes 1 and 4 both represent 4-connected sql net, 2 represents 6-connected pcu net, 3 exhibits a novel (3,12)-connected net, while 5 and 6 display (3,5)-connected gek1 net. The six complexes exhibit two kinds of inorganic–organic connectivities: I{sup 0}O{sup 2} for 1, 4–6, and I{sup 1}O{sup 2} for 2–3. The photoluminescent properties of 4–5 and the magnetic properties of 6 have been investigated. - Graphical abstract: Six new Pb(II)/Cd(II)/Mn(II) coordination polymers with helical structures based on flexible V-shaped dicarboxylate ligand have been synthesized and structurally characterized. Photoluminescent and magnetic properties have been investigated. - Highlights: • Six novel M(II) coordination polymers with 2,2′-[hexafluoroisopropylidenebis(p-phenyleneoxy)]diacetic acid and N-donor ligands. • Complexes 1–6 show diverse intriguing helical characters. • The luminescent properties of complexes 1–5 were investigated. • Complex 6 shows antiferromagnetic coupling.

Two Iron Complexes as Homogeneous and Heterogeneous Catalysts for the Chemical Fixation of Carbon Dioxide.

Science.gov (United States)

Karan, Chandan Kumar; Bhattacharjee, Manish

2018-04-16

Two new bimetallic iron-alkali metal complexes of amino acid (serine)-based reduced Schiff base ligand were synthesized and structurally characterized. Their efficacy as catalysts for the chemical fixation of carbon dioxide was explored. The heterogeneous version of the catalytic reaction was developed by the immobilization of these homogeneous bimetallic iron-alkali metal complexes in an anion-exchange resin. The resin-bound complexes can be used as recyclable catalysts up to six cycles.

Ruthenium phosphine complexes as catalysts for alternating co-polymerization of ethylene and CO

International Nuclear Information System (INIS)

Gusev, O.V.; Kal'sin, A.M.; Peganov, T.A.; Petrovskij, P.V.; Belov, G.P.; Novikova, E.V.

2000-01-01

Ruthenium (2) complexes, [Ru(dppe) 2 (OTs) 2 ] and [Ru(PhP(CH 2 CH 2 CH 2 PPh 2 ) 2 )(OTs) 2 ], where dppe (diphenylphosphino)ethane; OTs = tosylate, were synthesized with the yield of 67 and 76%, respectively, and characterized by 31 P NMR. The properties of the above complexes as catalysts of alternating co-polymerization of ethylene and carbon monoxide were studied. A considerable increase in catalytic activity of the complexes was established in the presence of trifluoroacetic acid and 1,4-benzoquinone. These compounds are the first example of ruthenium complexes that catalyse co-polymerization of ethylene and CO [ru

SYNTHESIZER CONTROLLED BEAM TRANSFER FROM THE AGS TO RHIC

International Nuclear Information System (INIS)

DELONG, J.; BRENNAN, J.M.; FISCHER, W.; HAYES, T.; SMITH, K.; VALENTINO, S.

2001-01-01

To ensure minimal losses and to preserve longitudinal emittance, beam is transferred from the AGS to the RHIC bunch to bucket. This requires precision frequency and phase control for synchronization and kicker timing. The required precision is realized with a set of Direct Digital Synthesizers. Each synthesizer can be frequency and phase modulated to align the AGS bunch to the target bucket in the RHIC phase

Synthesis, thermodynamic properties and antibacterial activities of lanthanide complexes with 3,5-dimethoxybenzoic acid and 1,10-phenanthroline

Energy Technology Data Exchange (ETDEWEB)

Zheng, Jun-Ru [Testing and Analysis Center, Hebei Normal University, Shijiazhuang 050024 (China); College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China); Ren, Shu-Xia [Material Science and Engineering School, Shijiazhuang Tiedao University, Shijiazhaung 050043 (China); Ren, Ning [Department of Chemistry, Handan College, Handan 056005 (China); Zhang, Jian-Jun, E-mail: jjzhang6@126.com [Testing and Analysis Center, Hebei Normal University, Shijiazhuang 050024 (China); College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China); Zhang, Da-Hai [Department of Chemistry, Handan College, Handan 056005 (China); Wang, Shu-Ping [College of Chemistry and Material Science, Hebei Normal University, Shijiazhuang 050024 (China)

2013-11-20

Graphical abstract: Four novel complexes ([Ln(3,5-DmeoxBA){sub 3}(phen)]{sub 2} (Ln = Tb(1), Dy(2), Er(3), Yb(4); 3,5-DmeoxBA = 3,5-dimethoxybenzoic acid; phen = 1,10-phenanthroline))were synthesized and characterized by elemental analysis, IR and TG/DSC-FTIR technology. Heat capacities of the four complexes were measured by differential scanning calorimetry (DSC). The antibacterial action of the four complexes on bacteria and fungus such as Escherichia coli, Staphylococcus aureus and Candida albicans were studied by filter paper approach. - Highlights: • Four novel complexes ([Ln(3,5-DmeoxBA){sub 3}(phen)]{sub 2} were synthesized and characterized. • The thermal decomposition processes of the title complexes were studied using the TG/DSC–FTIR coupling techniques. • The heat capacities of the complexes were measured by (DSC). • The antibacterial action of the four complexes on Escherichia coli, Staphylococcus aureus and Candida albicans were studied. - Abstract: Four lanthanide complexes with a general formula [Ln(3,5-DmeoxBA){sub 3}(phen)]{sub 2} (Ln = Tb(1), Dy(2), Er(3), Yb(4); 3,5-DmeoxBA = 3,5-dimethoxybenzoic acid; phen = 1,10-phenanthroline) were synthesized and characterized by elemental analysis, infrared spectra (IR), and thermogravimetric, differential scanning calorimetry techniques, combined with Fourier transform infrared (TG/DSC–FTIR) technology. The thermal decomposition processes of the four complexes were investigated by TG/DSC–FTIR techniques. Heat capacities were measured by DSC. The values of the experimental heat capacities were fitted to a polynomial equation with the least-squares method. Based on the fitted polynomial, the smoothed heat capacities and thermodynamic functions (H{sub T} − H{sub 298.15} {sub K}), (S{sub T} − S{sub 298.15} {sub K}), and (G{sub T} − G{sub 298.15} {sub K}) were calculated. The antibacterial action of the four complexes on bacteria and fungus such as Escherichia coli, Staphylococcus aureus and

Synthesis of complex oxides with garnet structure by spray drying of an aqueous salt solution

Science.gov (United States)

Makeenko, A. V.; Larionova, T. V.; Klimova-Korsmik, O. G.; Starykh, R. V.; Galkin, V. V.; Tolochko, O. V.

2017-04-01

The use of spray drying to obtain powders of complex oxides with a garnet structure has demonstrated. The processes occurring during heating of the synthesized oxide-salt product, leading to the formation of a material with a garnet structure, have been investigated using DTA, TGA, XPS, and XRD. It has been shown that a single-phase garnet structure of system (Y x Gd(3- x))3Al5O12 can be synthesized over the entire range of compositions.

The Semi-automatic Synthesis of 18F-fluoroethyl-choline by Domestic FDG Synthesizer

Directory of Open Access Journals (Sweden)

ZHOU Ming

2016-02-01

Full Text Available As an important complementary imaging agent for 18F-FDG, 18F-fluoroethyl-choline (18F-FECH has been demonstrated to be promising in brain and prostate cancer imaging. By using domestic PET-FDG-TI-I CPCU synthesizer, 18F-FECH was synthesized by different reagents and consumable supplies. The C18 column was added before the product collection bottle to remove K2.2.2. The 18F-FECH was synthesized by PET-FDG-IT-I synthesizer efficiently about 30 minutes by radiochemical yield of 42.0% (no decay corrected, n=5, and the radiochemical purity was still more than 99.0% after 6 hours. The results showed the domestic PET-FDG-IT-I synthesizer could semi-automatically synthesize injectable 18F-FECH in high efficiency and radiochemical purity

Forward osmosis for oily wastewater reclamation: Multi-charged oxalic acid complexes as draw solutes.

Science.gov (United States)

Ge, Qingchun; Amy, Gary Lee; Chung, Tai-Shung

2017-10-01

Forward osmosis (FO) has demonstrated its merits in hybrid FO seawater desalination. However, FO may have a potential for other applications if suitable draw solutes are available. In this study, a series of novel draw solutes based on oxalic acid (OA)-transitional metal complexes are presented. Influential factors of FO performance have been systematically investigated by varying the transitional metals, cations of the complex draw solutes as well as the experimental conditions. Compared to NaCl and other recently synthesized draw solutes, the OA complexes show superior FO performance in terms of high water fluxes up to 27.5 and 89.1 LMH under the respective FO and PRO (pressure retarded osmosis) modes, both with negligible reverse solute fluxes. The features of octahedral geometry, abundant hydrophilic groups and ionic species are crucial for the OA complexes as appropriate draw solutes with satisfactory FO performance. Among the synthesized OA complexes, the ammonium salt of chromic complex (NH 4 -Cr-OA) outperforms others due to the presence of more ionic species in its complex system. NH 4 -Cr-OA also performs better than the typical NaCl draw solute in FO oily wastewater treatment with higher water recovery and negligible reverse fluxes. Dilute solutions of OA complexes have been reconcentrated through membrane distillation (MD) and reused to new round of FO processes. The OA complexes have demonstrated their suitability and superiority as a novel class of draw solutes for the FO process in this study. Copyright © 2017 Elsevier Ltd. All rights reserved.

Synthesis and Characterization of 4-Benzyloxybenzaldehyde-4-methyl-3-thiosemicarbazone (Containing Sulphur and Nitrogen Donor Atoms and Its Cd(II Complex

Directory of Open Access Journals (Sweden)

Lakshmi Narayana Suvarapu

2015-12-01

Full Text Available A chelating agent, 4-benzyloxybenzaldehyde-4-methyl-3-thiosemicarbazone (BBMTSC, containing sulphur and nitrogen donor atoms was synthesized and applied as a ligand for the chelation of Cd(II. Both the BBMTSC and its Cd(II complex were characterized by elemental analysis, UV-Vis absorption spectra, Fourier transform infrared spectroscopy (FT-IR, mass spectra, nuclear magnetic resonance spectroscopy (NMR, X-ray powder diffraction (XRD, and field emission scanning electron microscopy (FESEM. The FTIR spectra confirmed the formation of both BBMTSC and its Cd(II complex. XRD revealed the polycrystalline nature of the synthesized compounds. BBMTSC exhibited a flake-like micro-rod morphology, whereas the Cd(II complex had a flower-like nanorod structure.

Chemical reactivity of analogous technetium(V) and rhenium(V) dioxo complexes

International Nuclear Information System (INIS)

Kremer, C.; Kremer, E.; Leon, A.

1993-01-01

All complexes of the series [MO 2 L 2 ] + (M = Tc, Re, L = ethylenediamine (en), 1,3-diaminopropane (1,3-dap)) have been synthesized and their chemical reactivities investigated. The following properties were studied: stability of the aqueous solutions at different pH values, substitution kinetics, lipophilicity and protein binding. The complexes show very similar reactivity in aqueous solution. From a radiopharmaceutical point of view, no significant difference in their in vivo behavior is expected. (author) 12 refs.; 1 fig.; 3 tabs

Ruthenium (II) complexes of thiosemicarbazone: Synthesis, biosensor applications and evaluation as antimicrobial agents

Energy Technology Data Exchange (ETDEWEB)

Yildirim, Hatice [Dokuz Eylul University, The Graduate School of Natural and Applied Sciences, Department of Chemistry, 35160 Buca, Izmir (Turkey); Guler, Emine [Ege University, Faculty of Science, Department of Biochemistry, 35100 Bornova, Izmir (Turkey); Yavuz, Murat, E-mail: myavuz@dicle.edu.tr [Ege University, Faculty of Science, Department of Biochemistry, 35100 Bornova, Izmir (Turkey); Dicle University, Faculty of Science, Department of Chemistry, 21280 Diyarbakir (Turkey); Ozturk, Nurdan; Kose Yaman, Pelin [Dokuz Eylul University, The Graduate School of Natural and Applied Sciences, Department of Chemistry, 35160 Buca, Izmir (Turkey); Subasi, Elif; Sahin, Elif [Dokuz Eylul University, Faculty of Science, Department of Chemistry, 35160 Buca, Izmir (Turkey); Timur, Suna [Ege University, Faculty of Science, Department of Biochemistry, 35100 Bornova, Izmir (Turkey); Ege University, Institute on Drug Abuse, Toxicology and Pharmaceutical Science (BATI), 35100 Bornova, Izmir (Turkey)

2014-11-01

A conformationally rigid half-sandwich organoruthenium (II) complex [(η{sup 6}-p-cymene)RuClTSC{sup N–S}]Cl, (1) and carbonyl complex [Ru(CO)Cl(PPh{sub 3}){sub 2}TSC{sup N–S}] (2) have been synthesized from the reaction of [{(η"6-p-cymene)RuCl}{sub 2}(μ-Cl){sub 2}] and [Ru(H)(Cl)(CO)(PPh{sub 3}){sub 3}] with thiophene-2-carboxaldehyde thiosemicarbazon (TSC) respectively and both novel ruthenium (II) complexes have been characterized by elemental analysis, FT-IR and NMR spectroscopy. The peripheral TSC in the complexes acts as an electrochemical coupling unit providing the ability to carry out electrochemical deposition (ED) and to form an electro-deposited film on a graphite electrode surface. The biosensing applicability of complexes 1 and 2 was investigated by using glucose oxidase (GOx) as a model enzyme. Electrochemical measurements at − 0.9 V versus Ag/AgCl electrode by following the ED Ru(II) reduction/oxidation due to from the enzyme activity, in the presence of glucose substrate. The designed biosensor showed a very good linearity for 0.01–0.5 mM glucose. The in vitro antimicrobial activities of complexes 1 and 2 were also investigated against nine bacterial strains and one fungus by the disc diffusion test method. No activity was observed against the Gram-negative strains and fungus, whereas complex 1 showed moderate antibacterial activities against Gram-positive bacterial strains. - Highlights: • Novel Ru (II) thiosemicarbazone complexes were synthesized and characterized. • Electrochemical depositions were performed. • Rigid half-sandwich Ru (II) complex showed enhanced antibacterial activity.

Zinc Oxide Nano crystals Synthesized by Quenching Technique

International Nuclear Information System (INIS)

Norhayati Abu Bakar; Akrajas Ali Umar; Muhamad Mat Salleh; Muhammad Yahya

2011-01-01

This paper reports an attempt to synthesize non toxic zinc oxide (ZnO) nano crystals using a simple quenching technique. The hot zinc oxide powder was quenched in hexane solution to obtain ZnO nano crystals. As the result, diameter size of the synthesized ZnO is 200 nm. It was also exhibited a good crystalline with wurtzite phase. The nano crystals properties of ZnO were revealed from good absorbance and green luminescence under UV exposure. This may be related with oxygen vacancy ionization during the annealing process. (author)

Biological activities of synthesized silver nanoparticles

Indian Academy of Sciences (India)

The C. halicacabum leaf extract synthesized AgNPs efficiency were tested against different bacterial pathogens MTCC-426 Proteus vulgaris, MTCC-2453 Pseudomonas aeruginosa, MTCC-96 Staphylococcus aureus, MTCC-441 Bacillus subtilis andMTCC-735 Salmonella paratyphi, and fungal pathogens Alternaria solani ...

Gold-Catalyzed Enantio- and Diastereoselective Syntheses of Left Fragments of Azadirachtin/Meliacarpin-Type Limonoids.

Science.gov (United States)

Shi, Hang; Tan, Ceheng; Zhang, Weibin; Zhang, Zichun; Long, Rong; Gong, Jianxian; Luo, Tuoping; Yang, Zhen

2016-02-05

Meliacarpin-type limonoids are an important class of organic insecticides. Their syntheses are challenging due to their chemical complexity. Here, we report the highly enantio- and diastereoselective synthesis of the left fragments of azadirachtin I and 1-cinnamoylmelianolone, being two important family members of meliacarpin-type limonoids, via pairwise palladium- and gold-catalyzed cascade reactions. Gold-catalyzed reactions of 1,7-diynes were performed as model studies, and the efficient construction of tetracyclic late-stage intermediates was achieved on the basis of this key transformation. Our unique route gave both of the left fragments in 23 steps from the commercially available chiral starting material (-)-carvone. This study significantly advances research on the synthesis of the meliacarpin-type limonoids.

Synthesis, characterization and anticancer activity of kaempferol-zinc(II) complex.

Science.gov (United States)

Tu, Lv-Ying; Pi, Jiang; Jin, Hua; Cai, Ji-Ye; Deng, Sui-Ping

2016-06-01

According to the previous studies, the anticancer activity of flavonoids could be enhanced when they are coordinated with transition metal ions. In this work, kaempferol-zinc(II) complex (kaempferol-Zn) was synthesized and its chemical properties were characterized by UV-VIS, FT-IR, (1)H NMR, elemental analysis, electrospray mass spectrometry (ES-MS) and fluorescence spectroscopy, which showed that the synthesized complex was coordinated with a Zn(II) ion via the 3-OH and 4-oxo groups. The anticancer effects of kaempferol-Zn and free kaempferol on human oesophageal cancer cell line (EC9706) were compared. MTT results demonstrated that the killing effect of kaempferol-Zn was two times higher than that of free kaempferol. Atomic force microscopy (AFM) showed the morphological and ultrastructural changes of cellular membrane induced by kaempferol-Zn at subcellular or nanometer level. Moreover, flow cytometric analysis indicated that kaempferol-Zn could induce apoptosis in EC9706 cells by regulating intracellular calcium ions. Collectively, all the data showed that kaempferol-Zn might be served as a kind of potential anticancer agent. Copyright © 2016 Elsevier Ltd. All rights reserved.

Enzymatic synthesizing of phytosterol oleic esters.

Science.gov (United States)

Pan, Xinxin; Chen, Biqiang; Wang, Juan; Zhang, Xinzhi; Zhul, Biyun; Tan, Tianwei

2012-09-01

A method of synthesizing the phytosterol esters from oleic acid and sterols was studied, using immobilized lipase Candida sp. 99-125 as catalyst. Molar ratio (oleic acid/phytosterols), temperature, reaction period, organic solvents, catalyst, and silica-gel drier were optimized, and the result showed that 93.4% of the sterols had been esterified under the optimal synthetic condition: the molar ratio of oleic acid/phytosterol is 1:1 in 10 mL iso-octane, immobilized lipase (w, 140% of the sterols), incubated in an orbital shaker (200 rpm) at a temperature of 45 °C for 24 h. The immobilized lipase could be reused for at least 13 times with limited loss of esterification activity. The conversion still maintained up to 86.6%. Hence, this developed process for synthesizing phytosterol esters could be considered as simple and low-energy consumption compared to existing chemical processes.

Grafting of a novel gold(III) complex on nanoporous MCM-41 and evaluation of its toxicity in Saccharomyces cerevisiae.

Science.gov (United States)

Fazaeli, Yousef; Amini, Mostafa M; Ashourion, Hamed; Heydari, Homayoun; Majdabadi, Abbas; Jalilian, Amir Reza; Abolmaali, Shamsozoha

2011-01-01

The goal of this research was to investigate the potential of newly synthesized gold complex trichloro(2,4,6-trimethylpyridine)Au(III) as an anticancer agent. The gold(III) complex was synthesized and grafted on nanoporous silica, MCM-41, to produce AuCl(3)@PF-MCM- 41 (AuCl(3) grafted on pyridine-functionalized MCM-41). The toxicity of trichloro(2,4,6- trimethylpyridine)Au(III) and AuCl(3)@PF-MCM-41 in Saccharomyces cerevisiae (as a model system) was studied. The gold(III) complex showed a mid cytotoxic effect on yeast viability. Using the drug delivery system, nanoporous MCM-41, the gold(III) complex became a strong inhibitor for growth of yeast cells at a very low concentration. Furthermore, the animal tests revealed a high uptake of AuCl(3)@PF-MCM-41 in tumor cells. The stability of the compound was confirmed in human serum.

Synthesis, characterization and biological studies of 2-(4-nitrophenylamino-carbonyl)benzoic acid and its complexes with Cr(III), Co(II), Ni(II), Cu(II) and Zn(II)

International Nuclear Information System (INIS)

Imran, M; Nazir, S.; Latif, S.; Mahmood, Z.

2010-01-01

Cr(III), Co(II), Ni(II), Cu(II) and Zn(II) complexes of 2-(4-Nitrophenyl aminocarbonyl)benzoic acid were synthesized and characterized on the basis of physical, analytical and spectroscopic data. The ligands, as well as its metal complexes were checked for their in-vitro antimicrobial activity against three bacterial strains, Mycobacterium smegmatis, Escherichia coli, Pseudomonas aeuroginosa, and three fungal strains, Nigrospora oryzae, Aspergillus niger and Candida albicans. Disc diffusion method and Tube diffusion test were used for antibacterial and antifungal activities, respectively. The synthesized complexes only show significant antifungal activity but inactive for antibacterial, however, in general, the metal complexes were found to be more active against antimicrobial activities as compared to their un complexed ligand. (author)

Synthesis, spectral studies and biological evaluation of 2-aminonicotinic acid metal complexes

Science.gov (United States)

Nawaz, Muhammad; Abbasi, Muhammad Waseem; Hisaindee, Soleiman; Zaki, Muhammad Javed; Abbas, Hira Fatima; Mengting, Hu; Ahmed, M. Arif

2016-05-01

We synthesized 2-aminonicotinic acid (2-ANA) complexes with metals such as Co(II), Fe(III), Ni(II), Mn(II), Zn(II), Ag(I),Cr(III), Cd(II) and Cu(II) in aqueous media. The complexes were characterized and elucidated using FT-IR, UV-Vis, a fluorescence spectrophotometer and thermo gravimetric analysis (TGA). TGA data showed that the stoichiometry of complexes was 1:2 metal/ligand except for Ag(I) and Mn(II) where the ratio was 1:1. The metal complexes showed varied antibacterial, fungicidal and nematicidal activities. The silver and zinc complexes showed highest activity against Bacillus subtilis and Bacillus licheniformis respectively. Fusarium oxysporum was highly susceptible to nickel and copper complexes whereas Macrophomina phaseolina was completely inert to the complexes. The silver and cadmium complexes were effective against the root-knot nematode Meloidogyne javanica.

Rhenium (5) and molybdenum (5) complexes with 4',4''(5'')-ditretbutyldibenzo-24-crown-8

International Nuclear Information System (INIS)

Ashurova, N.Kh.; Yakubov, K.G.; Basitova, S.M.; Tashmukhamedova, A.K.; Sajfullina, N.Zh.

1989-01-01

Rhenium and molybdenum complexes in +5 oxidation degree with 4',4''(5'')-ditretbutyldibenzo-24-crown-8 (L) are synthesized with 75-95 % yield. Composition and structure of compounds produced are investigated using element analysis, conductometry, IR spectroscopy, thermogravimetry methods. Oxidation degree of complexer metal is determined. It is ascertained that the compound composition corresponds to the MOLX 3 formula, where M-Re, Mo; X-Cl - , Br -

Essential oils-oriented fenvalerate analogues: syntheses, characterization and biological evaluation

International Nuclear Information System (INIS)

Su, H.; Li, H.

2016-01-01

A series of essential oils oriented ester derivatives have been designed, synthesized and characterized based on the skeleton of fenvalerate. The preliminary bioassay results indicated that some of the newly synthesized compounds showed better insecticidal activities against Pyrausta nubilalis and Heliothis armigera than that of the control trans-prallethrin chloride. (author)

DNA binding and biological activity of mixed ligand complexes of Cu(II, Ni(II and Co(II with quinolones and N donor ligand

Directory of Open Access Journals (Sweden)

S.M M Akram

2015-10-01

Full Text Available  AbstractMixed ligand complexes of  Cu(II, Ni(II and Co(II have been synthesized by using levofloxacin and bipyridyl and characterized using spectral and analytical techniques. The binding behavior of the Ni(II and Cu(II complexes with herring sperm DNA(Hs-DNA were determined using electronic absorption titration, viscometric measurements and cyclic voltammetry measurements. The binding constant calculated  for Cu(II and Ni(II complexes are 2.0 x 104 and 4.0 x 104 M-1 respectively. Detailed analysis reveals that these metal complexes interact with DNA through intercalative binding mode. The nuclease activity of  Cu(II and Ni(II complexes with ct-DNA was carried out using agarose gel electrophoresis technique. The antioxidant activities for the synthesized complexes have been tested and the antibacterial activity for Ni(II complex was also checked.Key words: Intercalation, hypochromism, red shift and  peak potential.

Synthesis, Characterization, and Physicochemical Studies of Mixed Ligand Complexes of Inner Transition Metals with Lansoprazole and Cytosine

Directory of Open Access Journals (Sweden)

Sarika Verma

2013-01-01

Full Text Available Few complexes of inner transition metals [Th(IV, Ce(IV, Nd(III, Gd(III] have been synthesized by reacting their metal salts with lansoprazole, 2-([3-methyl-4-(2,2,2-trifluoroethoxypyridin-2-yl]methylsulfinyl-1H-benzoimidazole and cytosine. All the complexes were synthesized in ethanolic medium. The yield percentage rangs from 80 to 90%. The complexes are coloured solids. The complexes were characterized through elemental analyses, conductance measurements, and spectroscopic methods (FT IR, FAB Mass, 1H NMR and UV. An IR spectrum indicates that the ligand behaves as bidentate ligands. The metal complexes have been screened for their antifungal activity towards Aspergillus niger fungi. The interaction of inner transition metals with lansoprazole, in presence of cytosine, has also been investigated potentiometrically at two different temperatures 26±1°C and 36±1°C and at 0.1 M (KNO3 ionic strength. The stability constants of ternary complexes indicate the stability order as Th(IV < Ce(IV < Gd(III < Nd(III. logK values obtained are positive and suggest greater stabilization of ternary complexes. The values of thermodynamic parameters (free energy (ΔG, enthalpy (ΔH, and entropy (ΔS are also calculated.

GHz band frequency hopping PLL-based frequency synthesizers

Institute of Scientific and Technical Information of China (English)

XU Yong; WANG Zhi-gong; GUAN Yu; XU Zhi-jun; QIAO Lu-feng

2005-01-01

In this paper we describe a full-integrated circuit containing all building blocks of a completed PLL-based synthesizer except for low pass filter(LPF).The frequency synthesizer is designed for a frequency hopping (FH) transceiver operating up to 1.5 GHz as a local oscillator. The architecture of Voltage Controlled Oscillator (VCO) is optimized to get better performance, and a phase noise of -111.85-dBc/Hz @ 1 MHz and a tuning range of 250 MHz are gained at a centre frequency of 1.35 GHz.A novel Dual-Modulus Prescaler(DMP) is designed to achieve a very low jitter and a lower power.The settling time of PLL is 80 μs while the reference frequency is 400 KHz.This monolithic frequency synthesizer is to integrate all main building blocks of PLL except for the low pass filter,with a maximum VCO output frequency of 1.5 GHz,and is fabricated with a 0.18 μm mixed signal CMOS process. Low power dissipation, low phase noise, large tuning range and fast settling time are gained in this design.

Manganese (III) cyclam complexes with aqua, iodo, nitrito, perchlorato and acetic acid/acetato axial ligands

DEFF Research Database (Denmark)

Mossin, Susanne; Sørensen, Henning Osholm; Weihe, Høgni

2005-01-01

of the complexes as high-spin d(4) systems. trans-[Mn(cyclam)(OH2)(2)](CF3SO3)(3)center dot H2O is shown to be a convenient starting material for the syntheses of trans cyclam complexes. [Mn(cyclam)(CH3COO)(CH3COOH)](ClO4)(2) exhibits extremely short intermolecular hydrogen bonds resulting in a pseudo-chain...

Bicarbonate catalysis of exchange synthesis of [51Cr]Cr(III)-EDTA and other chromium complexes

International Nuclear Information System (INIS)

Aronson, F.L.; Strashun, A.M.; Lopez, C.; Steigman, J.

1993-01-01

Exchange syntheses of trivalent chromium complexes often require heating, thus limiting tagging of heat-sensitive biological compounds with 51 Cr. Bicarbonate at pH 6, accelerates the formation of mM Cr-EDTA. Accordingly, room temperature catalysis with [ 51 Cr]Cr(III) at 10 -7 -10 -8 M was investigated. Complexes were successfully formed with EDTA and iminodiacetic acid (electrophoretic analysis) and acetylacetone and tropolone (analyzed by chloroform extraction). The formation of these complexes normally requires extensive heating. (author)

Structural, thermal, morphological and biological studies of proton-transfer complexes formed from 4-aminoantipyrine with quinol and picric acid

Science.gov (United States)

Adam, Abdel Majid A.

2013-03-01

4-Aminoantipyrine (4AAP) is widely used in the pharmaceutical industry, biochemical experiments and environmental monitoring. However, residual amounts of 4AAP in the environment may pose a threat to human health. To provide basic data that can be used to extract or eliminate 4AAP from the environment, the proton-transfer complexes of 4AAP with quinol (QL) and picric acid (PA) were synthesized and spectroscopically investigated. The interactions afforded two new proton-transfer salts named 1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-aminium-4-hydroxyphenolate and 1,5-dimethyl-3-oxo-2-phenyl-2,3-dihydro-1H-pyrazol-4-aminium-2,4,6-trinitrophenolate for QL and PA, respectively, via a 1:1 stoichiometry. Elemental analysis (CHN), electronic absorption, spectrophotometric titration, IR, Raman, 1H NMR and X-ray diffraction were used to characterize the new products. The thermal stability of the synthesized CT complexes was investigated using thermogravimetric (TG) analyses, and the morphology and particle size of these complexes were obtained from scanning electron microscopy (SEM). It was found that PA and 4AAP immediately formed a yellow precipitate with a remarkable sponge-like morphology and good thermal stability up to 180 °C. Finally, the biological activities of the newly synthesized CT complexes were tested for their antibacterial and antifungal activities. The results indicated that the [(4AAP)(QL)] complex exhibited strong antimicrobial activities against various bacterial and fungal strains compared with standard drugs.

The synthesis of N-Zn, N-Cu complexes involving 2-amino pyridine ...

Indian Academy of Sciences (India)

amino pyridine and ethylenediamine ligands (1a-b and 2a-b) have been described. They were synthesized with a simple, one-pot method, and the crystal structures of 1a, 1b, 2a and 2b were determined by X-ray crystallography. The complexes ...

Nano-Ag complexes prepared by γ-radiolysis and their structures and physical properties

International Nuclear Information System (INIS)

Kim, Hwa-Jung; Choi, Seong-Ho; Park, Hae-Jun

2012-01-01

In this study, nano-silver (nano-Ag) complexes showing different properties have been synthesized as follows. Polypyrrolidone (PVP)-stabilized silver colloids (NAg), nano-Ag bound to silica (SiO 2 ) (NSS), and nano-Ag bound to a complex of SiO 2 and polyaniline (PANI) (NSSPAI) were prepared via γ-irradiation at room temperature. NAg and NSS used PVP as a colloidal stabilizer, while NSSPAI did not use PVP as a colloidal stabilizer. Interesting bonding properties occurred in the nano-Ag complex and anticipated structural changes were clearly shown through a surface analysis of x-ray photoelectron spectroscopy (XPS). The morphologies by field emission-scanning electron microscopy (FE-SEM) analysis showed that nano-Ag complexes have various particle sizes ranging from 10 to 30 nm. NSS (average, 10 nm) and NSSPAI (average, 30 nm) showed a uniformly spherical shape and size, while NAg did not. From the reflection peaks in the x-ray diffraction (XRD) patterns, surface crystallinity of the nano-Ag complexes was indicated to be in the same degree as that of NSSPAI>NSS>NAg. Also, in the contact angle (CA) determination, surface hydrophobicity of NSSPAI was stronger than those of NSS and NAg, relatively. The different nano-Ag complexes prepared by γ-irradiation can be applicable in various industry fields due to the increase in specific property. - Highlights: ► Nano-Ag complexes showing different properties have been synthesized via γ-irradiation. ► Nano-Ag colloid (NAg), nano-Ag bound to SiO 2 (NSS), nano-Ag bound to SiO 2 and PANI complex (NSSPAI). ► Nano-Ag complexes were the same based on Ag metal. ► Results clearly showed fascinating/different physical properties. ► Different nano-Ag complexes can be applicable in various industry fields.